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Sample records for high lateral-resolution xps

  1. Round robin: Quantitative lateral resolution of PHI XPS microprobes Quantum 2000/Quantera SXM

    International Nuclear Information System (INIS)

    Scheithauer, Uwe; Kolb, Max; Kip, Gerard A.M.; Naburgh, Emile; Snijders, J.H.M.

    2016-01-01

    Highlights: • The quantitative lateral resolution of 7 PHI XPS microprobes has been estimated in a round robin. • An ellipsoidally shaped quartz crystal monochromatizes the Alkα radiation and refocuses it from the Al anode to the sample surface. • The long tail contributions of the X-ray beam intensity distribution were measured using a new and innovative approach. • This quantitative lateral resolution has a significantly larger value than the nominal X-ray beam diameter. • The quantitative lateral resolution follows a trend in time: The newer the monochromator so much the better the quantitative lateral resolution. - Abstract: The quantitative lateral resolution is a reliable measure for the quality of an XPS microprobe equipped with a focused X-ray beam. It describes the long tail contributions of the X-ray beam intensity distribution. The knowledge of these long tail contributions is essential when judging on the origin of signals of XPS spectra recorded on small-sized features. In this round robin test the quantitative lateral resolution of 7 PHI XPS microprobes has been estimated. As expected, the quantitative lateral resolution has significantly larger values than the nominal X-ray beam diameter. The estimated values of the quantitative lateral resolution follow a trend in time: the newer the monochromator of an XPS microprobe so much the better the quantitative lateral resolution.

  2. Round robin: Quantitative lateral resolution of PHI XPS microprobes Quantum 2000/Quantera SXM

    Energy Technology Data Exchange (ETDEWEB)

    Scheithauer, Uwe, E-mail: scht.uhg@googlemail.com [82008 Unterhaching (Germany); Kolb, Max, E-mail: max.kolb@airbus.com [Airbus Group Innovations, TX2, 81663 Munich (Germany); Kip, Gerard A.M., E-mail: G.A.M.Kip@utwente.nl [Universiteit Twente, MESA+ Nanolab, Postbus 217, 7500AE Enschede (Netherlands); Naburgh, Emile, E-mail: e.p.naburgh@philips.com [Materials Analysis, Philips Innovation Services, High Tech Campus 11, 5656 AE Eindhoven (Netherlands); Snijders, J.H.M., E-mail: j.h.m.snijders@philips.com [Materials Analysis, Philips Innovation Services, High Tech Campus 11, 5656 AE Eindhoven (Netherlands)

    2016-07-15

    Highlights: • The quantitative lateral resolution of 7 PHI XPS microprobes has been estimated in a round robin. • An ellipsoidally shaped quartz crystal monochromatizes the Alkα radiation and refocuses it from the Al anode to the sample surface. • The long tail contributions of the X-ray beam intensity distribution were measured using a new and innovative approach. • This quantitative lateral resolution has a significantly larger value than the nominal X-ray beam diameter. • The quantitative lateral resolution follows a trend in time: The newer the monochromator so much the better the quantitative lateral resolution. - Abstract: The quantitative lateral resolution is a reliable measure for the quality of an XPS microprobe equipped with a focused X-ray beam. It describes the long tail contributions of the X-ray beam intensity distribution. The knowledge of these long tail contributions is essential when judging on the origin of signals of XPS spectra recorded on small-sized features. In this round robin test the quantitative lateral resolution of 7 PHI XPS microprobes has been estimated. As expected, the quantitative lateral resolution has significantly larger values than the nominal X-ray beam diameter. The estimated values of the quantitative lateral resolution follow a trend in time: the newer the monochromator of an XPS microprobe so much the better the quantitative lateral resolution.

  3. Applications of high lateral and energy resolution imaging XPS with a double hemispherical analyser based spectromicroscope

    International Nuclear Information System (INIS)

    Escher, M.; Winkler, K.; Renault, O.; Barrett, N.

    2010-01-01

    The design and applications of an instrument for imaging X-ray photoelectron spectroscopy (XPS) are reviewed. The instrument is based on a photoelectron microscope and a double hemispherical analyser whose symmetric configuration avoids the spherical aberration (α 2 -term) inherent for standard analysers. The analyser allows high transmission imaging without sacrificing the lateral and energy resolution of the instrument. The importance of high transmission, especially for highest resolution imaging XPS with monochromated laboratory X-ray sources, is outlined and the close interrelation of energy resolution, lateral resolution and analyser transmission is illustrated. Chemical imaging applications using a monochromatic laboratory Al Kα-source are shown, with a lateral resolution of 610 nm. Examples of measurements made using synchrotron and laboratory ultra-violet light show the broad field of applications from imaging of core level electrons with chemical shift identification, high resolution threshold photoelectron emission microscopy (PEEM), work function imaging and band structure imaging.

  4. Laser-induced local activation of Mg-doped GaN with a high lateral resolution for high power vertical devices

    Science.gov (United States)

    Kurose, Noriko; Matsumoto, Kota; Yamada, Fumihiko; Roffi, Teuku Muhammad; Kamiya, Itaru; Iwata, Naotaka; Aoyagi, Yoshinobu

    2018-01-01

    A method for laser-induced local p-type activation of an as-grown Mg-doped GaN sample with a high lateral resolution is developed for realizing high power vertical devices for the first time. As-grown Mg-doped GaN is converted to p-type GaN in a confined local area. The transition from an insulating to a p-type area is realized to take place within about 1-2 μm fine resolution. The results show that the technique can be applied in fabricating the devices such as vertical field effect transistors, vertical bipolar transistors and vertical Schottkey diode so on with a current confinement region using a p-type carrier-blocking layer formed by this technique.

  5. Lateral resolution of eddy current imaging

    International Nuclear Information System (INIS)

    Hassan, W.; Blodgett, M.; Nagy, P.B.

    2002-01-01

    Analytical, finite element simulation, and experimental methods were used to investigate the lateral resolution of eddy current microscopy. It was found that the lateral resolution of eddy current imaging is ultimately limited by the probe-coil geometry and dimensions, but both the inspection frequency and the phase angle can be used to optimize the resolution, to some degree, at the expense of sensitivity. Electric anisotropy exhibited by noncubic crystallographic classes of materials such as titanium alloys can play a very similar role in electromagnetic materials characterization of polycrystalline metals to that of elastic anisotropy in ultrasonic materials characterization. Our results demonstrate that eddy current microscopy can be enhanced via a high-resolution, small diameter probe-coil which delivers a unique materials characterization tool well suited for the evaluation of Ti alloys

  6. Quantitative XPS analysis of high Tc superconductor surfaces

    International Nuclear Information System (INIS)

    Jablonski, A.; Sanada, N.; Suzuki, Y.; Fukuda, Y.; Nagoshi, M.

    1993-01-01

    The procedure of quantitative XPS analysis involving the relative sensitivity factors is most convenient to apply to high T c superconductor surfaces because this procedure does not require standards. However, a considerable limitation of such an approach is its relatively low accuracy. In the present work, a proposition is made to use for this purpose a modification of the relative sensitivity factor approach accounting for the matrix and the instrumental effects. The accuracy of this modification when applied to the binary metal alloys is 2% or better. A quantitative XPS analysis was made for surfaces of the compounds Bi 2 Sr 2 CuO 6 , Bi 2 Sr 2 CaCu 2 O 8 , and YBa 2 Cu 3 O Y . The surface composition determined for the polycrystalline samples corresponds reasonably well to the bulk stoichiometry. Slight deficiency of oxygen was found for the Bi-based compounds. The surface exposed on cleavage of the Bi 2 Sr 2 CaCu 2 O 8 single crystal was found to be enriched with bismuth, which indicates that the cleavage occurs along the BiO planes. This result is in agreement with the STM studies published in the literature

  7. 'Applications of stable isotopes in life sciences'. Lead and strontium stable isotope measurements by using a high lateral resolution secondary ion mass spectrometer (NanoSIMS)

    International Nuclear Information System (INIS)

    Sano, Yuji

    2008-01-01

    The method of Pb and Sr isotope measurements at about 5 μm resolution was developed by using a high lateral resolution secondary ion mass spectrometer (NanoSIMS NS50). Since the both elements have radiogenic nuclides such as 206 Pb, 207 Pb, and 87 Sr, natural variations of isotopic ratios are large. It is possible to detect a meaningful variation in a terrestrial sample, even though the experimental error is relatively large. In the case of monazite U-Pb dating, a 4 nA O - primary beam was used to sputter the sample and secondary positive ions were extracted for mass analysis using a Mattauch-Herzog geometry. The multi-collector system was modified to detect 140 Ce + , 204 Pb + , 206 Pb + , 238 U 16 O + , and 238 U 16 O 2 + ions simultaneously. Based on the monazite standard from North-Central Madagascar, we have determined the 206 Pb/ 238 U ratios of samples. 207 Pb/ 206 Pb ratios were measured by a magnet scanning with a single collector mode. 44 monazite grains extracted from a sedimentary rock in Taiwan were analyzed. Observed ages were consistent with the U-Th-Pb chemical ages by EPMA. Then NanoSIMS has been used to measure 87 Sr/ 86 Sr ratios in natural calcium carbonate samples. Multi-collector system was adjusted to detect 43 Ca + , 80 Ca 2 + , 86 Sr + , and 87 Sr + ions at the same time. Magnetic field was scanning for the EM no.4 counter to detect 85 Rb + , 86 Sr + and 87 Sr + , while the EM no.4b can measure 86 Sr + , 87 Sr + , and 88 Sr + , respectively. Repeated analyses of a coral skeleton standard (JCp-1) show that 87 Sr/ 86 Sr ratio agrees well with the seawater signature, after the series of corrections such as Ca dimer, 87 Rb, and a mass bias estimated by 88 Sr/ 86 Sr ratio. The method is applied to an otolith from ayu (Pleco-glossus altivelis altivelis) collected from the Yodo river, Japan. The spatial variation of 87 Sr/ 86 Sr ratios was consistent with amphidromous migration of the fish, namely, born in the lake and grown in the coastal sea

  8. Low voltage EPMA: experiments on a new frontier in microanalysis - analytical lateral resolution

    International Nuclear Information System (INIS)

    Fournelle, J; Cathey, H; Pinard, P T; Richter, S

    2016-01-01

    Field emission (FE) electron gun sources provide new capabilities for high lateral resolution EPMA. The determination of analytical lateral resolution is not as straightforward as that for electron microscopy imaging. Results from two sets of experiments to determine the actual lateral resolution for accurate EPMA are presented for Kα X-ray lines of Si and Al and La of Fe at 5 and 7 keV in a silicate glass. These results are compared to theoretical predictions and Monte Carlo simulations of analytical lateral resolution. The experiments suggest little is gained in lateral resolution by dropping from 7 to 5 keV in EPMA of this silicate glass. (paper)

  9. Valence band structure of binary chalcogenide vitreous semiconductors by high-resolution XPS

    International Nuclear Information System (INIS)

    Kozyukhin, S.; Golovchak, R.; Kovalskiy, A.; Shpotyuk, O.; Jain, H.

    2011-01-01

    High-resolution X-ray photoelectron spectroscopy (XPS) is used to study regularities in the formation of valence band electronic structure in binary As x Se 100−x , As x S 100−x , Ge x Se 100−x and Ge x S 100−x chalcogenide vitreous semiconductors. It is shown that the highest occupied energetic states in the valence band of these materials are formed by lone pair electrons of chalcogen atoms, which play dominant role in the formation of valence band electronic structure of chalcogen-rich glasses. A well-expressed contribution from chalcogen bonding p electrons and more deep s orbitals are also recorded in the experimental valence band XPS spectra. Compositional dependences of the observed bands are qualitatively analyzed from structural and compositional points of view.

  10. Valence band structure of binary chalcogenide vitreous semiconductors by high-resolution XPS

    Energy Technology Data Exchange (ETDEWEB)

    Kozyukhin, S., E-mail: sergkoz@igic.ras.ru [Russian Academy of Science, Institute of General and Inorganic Chemistry (Russian Federation); Golovchak, R. [Lviv Scientific Research Institute of Materials of SRC ' Carat' (Ukraine); Kovalskiy, A. [Lehigh University, Department of Materials Science and Engineering (United States); Shpotyuk, O. [Lviv Scientific Research Institute of Materials of SRC ' Carat' (Ukraine); Jain, H. [Lehigh University, Department of Materials Science and Engineering (United States)

    2011-04-15

    High-resolution X-ray photoelectron spectroscopy (XPS) is used to study regularities in the formation of valence band electronic structure in binary As{sub x}Se{sub 100-x}, As{sub x}S{sub 100-x}, Ge{sub x}Se{sub 100-x} and Ge{sub x}S{sub 100-x} chalcogenide vitreous semiconductors. It is shown that the highest occupied energetic states in the valence band of these materials are formed by lone pair electrons of chalcogen atoms, which play dominant role in the formation of valence band electronic structure of chalcogen-rich glasses. A well-expressed contribution from chalcogen bonding p electrons and more deep s orbitals are also recorded in the experimental valence band XPS spectra. Compositional dependences of the observed bands are qualitatively analyzed from structural and compositional points of view.

  11. XPS and FTIR spectroscopic study on microwave treated high phosphorus iron ore

    International Nuclear Information System (INIS)

    Omran, Mamdouh; Fabritius, Timo; Elmahdy, Ahmed M.; Abdel-Khalek, Nagui A.; El-Aref, Mortada; Elmanawi, Abd El-Hamid

    2015-01-01

    Highlights: • The effect of microwave radiation on structure and chemical state of high phosphorus iron ore was studied. • FTIR analyses showed that after microwave radiation the functional chemical groups of phosphorus bearing minerals (fluorapatite) dissociated. • High resolution XPS analyses of Fe 2p peaks showed that after microwave radiation a portion of Fe(+III) was reduced to Fe(+II). • Microwave radiation had a positive effect on the magnetic properties of iron oxide, through formation of ferromagnetic phases. - Abstract: A growing interest in microwave heating has emerged recently. Several potential microwave applications regarding minerals’ processing have been investigated. This paper investigates the effect of microwave radiation on Egyptian high phosphorus iron ore. Three different iron ore samples have varying Fe 2 O 3 and P 2 O 5 contents and mineralogical textures were studied. A comparative study has been carried out between untreated and microwave treated iron ore. XRD and FTIR analyses showed that after microwave radiation the crystallinity of iron bearing minerals (hematite) increased, while the functional chemical groups of phosphorus bearing minerals (fluorapatite) and other gangues dissociated. High resolution XPS analyses of Fe 2p peaks showed that after microwave radiation a portion of Fe(+III) was reduced to Fe(+II). This means that after microwave radiation iron oxide (hematite, Fe 3+ ) transformed into more magnetic phase. The results indicated that microwave radiation had a positive effect on the magnetic properties of iron oxide, through formation of ferromagnetic phases

  12. Characterization of Desulfovibrio desulfuricans biofilm on high-alloyed stainless steel: XPS and electrochemical studies

    Energy Technology Data Exchange (ETDEWEB)

    Dec, Weronika [Institute of Industrial Organic Chemistry, Branch Pszczyna, Doświadczalna Street 27, 43-200 Pszczyna (Poland); Mosiałek, Michał; Socha, Robert P. [Jerzy Haber Institute of Catalysis and Surface Chemistry PAS, Niezapominajek Street 8, 30-239 Kraków (Poland); Jaworska-Kik, Marzena [Department of Biopharmacy, Medical University of Silesia, Jedności Street 8, 41-200 Sosnowiec (Poland); Simka, Wojciech [Faculty of Chemistry, Silesian University of Technology, B. Krzywoustego 6 Street, 44-100 Gliwice (Poland); Michalska, Joanna, E-mail: joanna.k.michalska@polsl.pl [Faculty of Chemistry, Silesian University of Technology, B. Krzywoustego 6 Street, 44-100 Gliwice (Poland)

    2017-07-01

    Results on D. desulfuricans biofilm formation on austenitic-ferritic duplex (2205 DSS) and superaustenitic (904L) stainless steels are presented. Surface characterization including the structure, configuration and chemical composition of biofilms were carried out using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Electrochemical impedance spectroscopy (EIS) measurements were used to monitor the attachment activity of bacteria on the steels' surface and to determine the effect of bacteria on passivity. It was proved that investigated steels are rapidly colonized by bacteria. The presence of biofilm caused significant ennoblement of 904L steel surface, while retarded the attainment of high passive state of 2205 DSS. XPS analysis revealed significant sulphidation of the biofilm and its layered structure. Accumulation of sulphides and hydroxides was proved in the outermost layer, while the increasing contents of disulphides, organometallic and C-N bonds were detected in the internal part of the biofilm. Irreversible bondings between steel matrix and biofilm had also been observed. - Highlights: • High-alloyed steels are rapidly colonized by sulphate-reducing bacteria. • Higher Ni content stimulates more intensive biofilm growth. • Extracellular polymeric substances indelibly bind to the high-alloyed steels. • Sulphate-reducing bacteria caused irreversible sulphidation of passive films.

  13. Characterization of Desulfovibrio desulfuricans biofilm on high-alloyed stainless steel: XPS and electrochemical studies

    International Nuclear Information System (INIS)

    Dec, Weronika; Mosiałek, Michał; Socha, Robert P.; Jaworska-Kik, Marzena; Simka, Wojciech; Michalska, Joanna

    2017-01-01

    Results on D. desulfuricans biofilm formation on austenitic-ferritic duplex (2205 DSS) and superaustenitic (904L) stainless steels are presented. Surface characterization including the structure, configuration and chemical composition of biofilms were carried out using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Electrochemical impedance spectroscopy (EIS) measurements were used to monitor the attachment activity of bacteria on the steels' surface and to determine the effect of bacteria on passivity. It was proved that investigated steels are rapidly colonized by bacteria. The presence of biofilm caused significant ennoblement of 904L steel surface, while retarded the attainment of high passive state of 2205 DSS. XPS analysis revealed significant sulphidation of the biofilm and its layered structure. Accumulation of sulphides and hydroxides was proved in the outermost layer, while the increasing contents of disulphides, organometallic and C-N bonds were detected in the internal part of the biofilm. Irreversible bondings between steel matrix and biofilm had also been observed. - Highlights: • High-alloyed steels are rapidly colonized by sulphate-reducing bacteria. • Higher Ni content stimulates more intensive biofilm growth. • Extracellular polymeric substances indelibly bind to the high-alloyed steels. • Sulphate-reducing bacteria caused irreversible sulphidation of passive films.

  14. XPS and FTIR spectroscopic study on microwave treated high phosphorus iron ore

    Energy Technology Data Exchange (ETDEWEB)

    Omran, Mamdouh, E-mail: mamdouh.omran@oulu.fi [Process Metallurgy Research Group, Faculty of Technology, University of Oulu (Finland); Mineral Processing and Agglomeration Lab, Central Metallurgical Research and Development Institute, Cairo (Egypt); Fabritius, Timo [Process Metallurgy Research Group, Faculty of Technology, University of Oulu (Finland); Elmahdy, Ahmed M.; Abdel-Khalek, Nagui A. [Mineral Processing and Agglomeration Lab, Central Metallurgical Research and Development Institute, Cairo (Egypt); El-Aref, Mortada; Elmanawi, Abd El-Hamid [Geology Department, Faculty of Science, Cairo University, Giza 12613 (Egypt)

    2015-08-01

    Highlights: • The effect of microwave radiation on structure and chemical state of high phosphorus iron ore was studied. • FTIR analyses showed that after microwave radiation the functional chemical groups of phosphorus bearing minerals (fluorapatite) dissociated. • High resolution XPS analyses of Fe 2p peaks showed that after microwave radiation a portion of Fe(+III) was reduced to Fe(+II). • Microwave radiation had a positive effect on the magnetic properties of iron oxide, through formation of ferromagnetic phases. - Abstract: A growing interest in microwave heating has emerged recently. Several potential microwave applications regarding minerals’ processing have been investigated. This paper investigates the effect of microwave radiation on Egyptian high phosphorus iron ore. Three different iron ore samples have varying Fe{sub 2}O{sub 3} and P{sub 2}O{sub 5} contents and mineralogical textures were studied. A comparative study has been carried out between untreated and microwave treated iron ore. XRD and FTIR analyses showed that after microwave radiation the crystallinity of iron bearing minerals (hematite) increased, while the functional chemical groups of phosphorus bearing minerals (fluorapatite) and other gangues dissociated. High resolution XPS analyses of Fe 2p peaks showed that after microwave radiation a portion of Fe(+III) was reduced to Fe(+II). This means that after microwave radiation iron oxide (hematite, Fe{sup 3+}) transformed into more magnetic phase. The results indicated that microwave radiation had a positive effect on the magnetic properties of iron oxide, through formation of ferromagnetic phases.

  15. A novel ToF-SIMS operation mode for sub 100 nm lateral resolution: Application and performance

    International Nuclear Information System (INIS)

    Kubicek, Markus; Holzlechner, Gerald; Opitz, Alexander K.; Larisegger, Silvia; Hutter, Herbert; Fleig, Jürgen

    2014-01-01

    A novel operation mode for time of flight-secondary ion mass spectrometry (ToF-SIMS) is described for a TOF.SIMS 5 instrument with a Bi-ion gun. It features sub 100 nm lateral resolution, adjustable primary ion currents and the possibility to measure with high lateral resolution as well as high mass resolution. The adjustment and performance of the novel operation mode are described and compared to established ToF-SIMS operation modes. Several examples of application featuring novel scientific results show the capabilities of the operation mode in terms of lateral resolution, accuracy of isotope analysis of oxygen, and combination of high lateral and mass resolution. The relationship between high lateral resolution and operation of SIMS in static mode is discussed.

  16. A novel ToF-SIMS operation mode for sub 100 nm lateral resolution: Application and performance.

    Science.gov (United States)

    Kubicek, Markus; Holzlechner, Gerald; Opitz, Alexander K; Larisegger, Silvia; Hutter, Herbert; Fleig, Jürgen

    2014-01-15

    A novel operation mode for time of flight-secondary ion mass spectrometry (ToF-SIMS) is described for a TOF.SIMS 5 instrument with a Bi-ion gun. It features sub 100 nm lateral resolution, adjustable primary ion currents and the possibility to measure with high lateral resolution as well as high mass resolution. The adjustment and performance of the novel operation mode are described and compared to established ToF-SIMS operation modes. Several examples of application featuring novel scientific results show the capabilities of the operation mode in terms of lateral resolution, accuracy of isotope analysis of oxygen, and combination of high lateral and mass resolution. The relationship between high lateral resolution and operation of SIMS in static mode is discussed.

  17. XPS analysis for cubic boron nitride crystal synthesized under high pressure and high temperature using Li3N as catalysis

    International Nuclear Information System (INIS)

    Guo, Xiaofei; Xu, Bin; Zhang, Wen; Cai, Zhichao; Wen, Zhenxing

    2014-01-01

    Highlights: • The cBN was synthesized by Li 3 N as catalyst under high pressure and high temperature (HPHT). • The film coated on the as-grown cBN crystals was studied by XPS. • The electronic structure variation in the film was investigated. • The growth mechanism of cubic boron nitride crystal was analyzed briefly. - Abstract: Cubic boron nitride (cBN) single crystals are synthesized with lithium nitride (Li3N) as catalyst under high pressure and high temperature. The variation of electronic structures from boron nitride of different layers in coating film on the cBN single crystal has been investigated by X-ray photoelectron spectroscopy. Combining the atomic concentration analysis, it was shown that from the film/cBN crystal interface to the inner, the sp 2 fractions are decreasing, and the sp 3 fractions are increasing in the film at the same time. Moreover, by transmission electron microscopy, a lot of cBN microparticles are found in the interface. For there is no Li 3 N in the film, it is possible that Li 3 N first reacts with hexagonal boron nitride to produce Li 3 BN 2 during cBN crystals synthesis under high pressure and high temperature (HPHT). Boron and nitrogen atoms, required for cBN crystals growth, could come from the direct conversion from hexagonal boron nitride with the catalysis of Li 3 BN 2 under high pressure and high temperature, but not directly from the decomposition of Li 3 BN 2

  18. A XPS study of the Mo effect on passivation behaviors for highly controlled stainless steels in neutral and alkaline conditions

    International Nuclear Information System (INIS)

    Mesquita, Thiago J.; Chauveau, Eric; Mantel, Marc; Nogueira, Ricardo P.

    2013-01-01

    The objective of this work is to study the effect of Mo additions on film passive properties of three different stainless steels (SS) types (austenitic, ferritic and duplex alloys). A comparison between Mo containing (3 wt% Mo) and free Mo (0 wt% Mo) grades of highly controlled laboratory heats was done considering their passive film formed in different aggressive conditions, from neutral to alkaline pH. The presence of oxidized Mo on the passive layer was confirmed by X-ray photoelectron Spectroscopy (XPS). The presence of Mo within the passive film improved the passivity breakdown potential for the duplex and ferritic SS, but seemed to have no effect for austenitic SS.

  19. A XPS study of the Mo effect on passivation behaviors for highly controlled stainless steels in neutral and alkaline conditions

    Energy Technology Data Exchange (ETDEWEB)

    Mesquita, Thiago J., E-mail: thiago.mesquita@ugitech.com [Ugitech Research Center, Avenue Paul Girod, 73403 Ugine Cedex (France); Chauveau, Eric; Mantel, Marc [Ugitech Research Center, Avenue Paul Girod, 73403 Ugine Cedex (France); Nogueira, Ricardo P. [LEPMI UMR 5279 CNRS – Grenoble INP–Université de Savoie–Université Joseph Fourier BP 75, 38402 St Martin d’Hères (France)

    2013-04-01

    The objective of this work is to study the effect of Mo additions on film passive properties of three different stainless steels (SS) types (austenitic, ferritic and duplex alloys). A comparison between Mo containing (3 wt% Mo) and free Mo (0 wt% Mo) grades of highly controlled laboratory heats was done considering their passive film formed in different aggressive conditions, from neutral to alkaline pH. The presence of oxidized Mo on the passive layer was confirmed by X-ray photoelectron Spectroscopy (XPS). The presence of Mo within the passive film improved the passivity breakdown potential for the duplex and ferritic SS, but seemed to have no effect for austenitic SS.

  20. Combining Raman Microprobe and XPS to Study High Temperature Oxidation of Metals

    International Nuclear Information System (INIS)

    Windisch, Charles F.; Henager, Charles H.; Engelhard, Mark H.; Bennett, Wendy D.

    2011-01-01

    Raman microprobe spectroscopy was applied in studies of high-temperature air oxidation of a ferritic alloy (HT-9) in the absence and presence of zirconia coatings with the objective of evaluating the technique as a way to quickly screen candidate cladding materials and actinide-based mixed oxide fuel mixtures for advanced nuclear reactors. When oxidation was relatively uniform, Raman spectra collected using microscope optics with low spatial resolution were found to be similar to those collected with conventional Raman spectroscopy. These spectra could be used to identify major oxide corrosion products and follow changes in the composition of the oxides due to heating. However, when the oxidation films were comprised of multiple layers of varying composition, or with layers containing metallic phases, techniques with higher depth resolution and sensitivity to zero-valence metals were necessary. The requirements were met by combining Raman microprobe using different optical configurations and x-ray photoelectron spectroscopy.

  1. Angle-dependent XPS study of the mechanisms of 'high-low temperature' activation of GaAs photocathode

    International Nuclear Information System (INIS)

    Du Xiaoqing; Chang Benkang

    2005-01-01

    The surface chemical compositions, atomic concentration percentage and layer thickness after 'high-temperature' single-step activation and 'high-low temperature' two-step activation were obtained using quantitative analysis of angle-dependent X-ray photoelectron spectroscopy (XPS). It was found that compared to single-step activation, the thickness of GaAs-O interface barrier had a remarkable decrease, the degree of As-O bond became much smaller and the Ga-O bond became dominating, and at the same time the thickness of (Cs, O) layer also had a deduction while the ratio of Cs to O had no change after two-step activation. The measured spectral response curves showed that a increase of 29% of sensitivity had been obtained after two-step activation. To explore the inherent mechanisms of influences of the evolution of GaAs(Cs, O) surface layers on photoemission, surface electric barrier models based on the experimental results were built. By calculation of electron escape probability it was found that the decrease of thickness of GaAs-O interface barrier and (Cs, O) layer is the main reasons, which explained why higher sensitivity is achieved after two-step activation than single-step activation

  2. Digital adaptive optics for achieving space-invariant lateral resolution in optical coherence tomography

    International Nuclear Information System (INIS)

    Kumar, A.

    2015-01-01

    Optical coherence tomography (OCT) is a non-invasive optical interferometric imaging technique that provides reflectivity profiles of the sample structures with high axial resolution. The high axial resolution is due to the use of low coherence (broad-band) light source. However, the lateral resolution in OCT depends on the numerical aperture (NA) of the focusing/imaging optics and it is affected by defocus and other higher order optical aberrations induced by the imperfect optics, or by the sample itself.Hardware based adaptive optics (AO) has been successfully combined with OCT to achieve high lateral resolution in combination with high axial resolution provided by OCT. AO, which conventionally uses Shack-Hartmann wavefront sensor (SH WFS) and deformable mirror for wavefront sensing and correction respectively, can compensate for optical aberration and can enable diffraction-limited resolution in OCT. Visualization of cone photoreceptors in 3-D has been successfully demonstrated using AO-OCT. However, OCT being an interferometric imaging technique can provide access to phase information.This phase information can be exploited by digital adaptive optics (DAO) techniques to correct optical aberration in the post-processing step to obtain diffraction-limited space invariant lateral resolution throughout the image volume. Thus, the need for hardware based AO can be eliminated, which in turn can reduce the system complexity and economical cost. In the first paper of this thesis, a novel DAO method based on sub-aperture correlation is presented which is the digital equivalent of SH WFS. The advantage of this method is that it is non-iterative in nature and it does not require a priori knowledge of any system parameters such wavelength, focal length, NA or detector pixel size. For experimental proof, a FF SS OCT system was used and the sample consisted of resolution test target and a plastic plate that introduced random optical aberration. Experimental results show that

  3. Improving lateral resolution and image quality of optical coherence tomography by the multi-frame superresolution technique for 3D tissue imaging.

    Science.gov (United States)

    Shen, Kai; Lu, Hui; Baig, Sarfaraz; Wang, Michael R

    2017-11-01

    The multi-frame superresolution technique is introduced to significantly improve the lateral resolution and image quality of spectral domain optical coherence tomography (SD-OCT). Using several sets of low resolution C-scan 3D images with lateral sub-spot-spacing shifts on different sets, the multi-frame superresolution processing of these sets at each depth layer reconstructs a higher resolution and quality lateral image. Layer by layer processing yields an overall high lateral resolution and quality 3D image. In theory, the superresolution processing including deconvolution can solve the diffraction limit, lateral scan density and background noise problems together. In experiment, the improved lateral resolution by ~3 times reaching 7.81 µm and 2.19 µm using sample arm optics of 0.015 and 0.05 numerical aperture respectively as well as doubling the image quality has been confirmed by imaging a known resolution test target. Improved lateral resolution on in vitro skin C-scan images has been demonstrated. For in vivo 3D SD-OCT imaging of human skin, fingerprint and retina layer, we used the multi-modal volume registration method to effectively estimate the lateral image shifts among different C-scans due to random minor unintended live body motion. Further processing of these images generated high lateral resolution 3D images as well as high quality B-scan images of these in vivo tissues.

  4. Numerical study of the lateral resolution in electrostatic force microscopy for dielectric samples

    International Nuclear Information System (INIS)

    Riedel, C; AlegrIa, A; Colmenero, J; Schwartz, G A; Saenz, J J

    2011-01-01

    We present a study of the lateral resolution in electrostatic force microscopy for dielectric samples in both force and gradient modes. Whereas previous studies have reported expressions for metallic surfaces having potential heterogeneities (Kelvin probe force microscopy), in this work we take into account the presence of a dielectric medium. We introduce a definition of the lateral resolution based on the force due to a test particle being either a point charge or a polarizable particle on the dielectric surface. The behaviour has been studied over a wide range of typical experimental parameters: tip-sample distance (1-20) nm, sample thickness (0-5) μm and dielectric constant (1-20), using the numerical simulation of the equivalent charge method. For potential heterogeneities on metallic surfaces expressions are in agreement with the bibliography. The lateral resolution of samples having a dielectric constant of more than 10 tends to metallic behaviour. We found a characteristic thickness of 100 nm, above which the lateral resolution measured on the dielectric surface is close to that of an infinite medium. As previously reported, the lateral resolution is better in the gradient mode than in the force mode. Finally, we showed that for the same experimental conditions, the lateral resolution is better for a polarizable particle than for a charge, i.e. dielectric heterogeneities should always look 'sharper' (better resolved) than inhomogeneous charge distributions. This fact should be taken into account when interpreting images of heterogeneous samples.

  5. Numerical study of the lateral resolution in electrostatic force microscopy for dielectric samples

    Energy Technology Data Exchange (ETDEWEB)

    Riedel, C; AlegrIa, A; Colmenero, J [Departamento de Fisica de Materiales UPV/EHU, Facultad de Quimica, Apartado 1072, 20080 San Sebastian (Spain); Schwartz, G A [Centro de Fisica de Materiales CSIC-UPV/EHU, Paseo Manuel de Lardizabal 5, 20018 San Sebastian (Spain); Saenz, J J, E-mail: riedel@ies.univ-montp2.fr [Donostia International Physics Center, Paseo Manuel de Lardizabal 4, 20018 San Sebastian (Spain)

    2011-07-15

    We present a study of the lateral resolution in electrostatic force microscopy for dielectric samples in both force and gradient modes. Whereas previous studies have reported expressions for metallic surfaces having potential heterogeneities (Kelvin probe force microscopy), in this work we take into account the presence of a dielectric medium. We introduce a definition of the lateral resolution based on the force due to a test particle being either a point charge or a polarizable particle on the dielectric surface. The behaviour has been studied over a wide range of typical experimental parameters: tip-sample distance (1-20) nm, sample thickness (0-5) {mu}m and dielectric constant (1-20), using the numerical simulation of the equivalent charge method. For potential heterogeneities on metallic surfaces expressions are in agreement with the bibliography. The lateral resolution of samples having a dielectric constant of more than 10 tends to metallic behaviour. We found a characteristic thickness of 100 nm, above which the lateral resolution measured on the dielectric surface is close to that of an infinite medium. As previously reported, the lateral resolution is better in the gradient mode than in the force mode. Finally, we showed that for the same experimental conditions, the lateral resolution is better for a polarizable particle than for a charge, i.e. dielectric heterogeneities should always look 'sharper' (better resolved) than inhomogeneous charge distributions. This fact should be taken into account when interpreting images of heterogeneous samples.

  6. Imaging modes for potential mapping in semiconductor devices by electron holography with improved lateral resolution

    Energy Technology Data Exchange (ETDEWEB)

    Sickmann, Jan, E-mail: jan.sickmann@triebenberg.de [Triebenberg Laboratory, Institute of Structure Physics, Technische Universitaet Dresden, 01069 Dresden (Germany); Formanek, Petr; Linck, Martin [Triebenberg Laboratory, Institute of Structure Physics, Technische Universitaet Dresden, 01069 Dresden (Germany); Muehle, Uwe [Institut fuer Werkstoffwissenschaft, Technische Universitaet Bergakademie Freiberg, 09599 Freiberg (Germany); Lichte, Hannes [Triebenberg Laboratory, Institute of Structure Physics, Technische Universitaet Dresden, 01069 Dresden (Germany)

    2011-03-15

    Electron holography is the highest resolving tool for dopant profiling at nanometre-scale resolution. In order to measure the object areas of interest in a hologram, both a wide field of view and a sufficient lateral resolution are required. The usual path of rays for recording holograms with an electron biprism using the standard objective lens does not meet these requirements, because the field of view amounts to some 10 nm only, however, at a resolution of 0.1 nm better than needed here. Therefore, instead of the standard objective lens, the Lorentz lens is widely used for holography of semiconductors, since it provides a field of view up to 1000 nm at a sufficient lateral resolution of about 10 nm. Since the size of semiconductor structures is steadily shrinking, there is now a need for better lateral resolution at an appropriate field of view. Therefore, additional paths of rays for recording holograms are studied with special emphasis on the parameters field of view and lateral resolution. The findings allow an optimized scheme with a field of view of 200 nm and a lateral resolution of 3.3 nm filling the gap between the existing set-ups. In addition, the Lorentz lens is no longer required for investigation of non-magnetic materials, since the new paths of rays are realized with the standard objective lens and diffraction lens. An example proves the applicability of this arrangement for future semiconductor technology. -- Research highlights: {yields} Imaging modes for potential mapping in semiconductor devices by electron holography. {yields} Using objective and diffraction lens for imaging instead of Lorentz lens. {yields} Detailed investigation of four different paths of rays and its basic parameters for holographic application: field of view, lateral resolution, signal resolution. {yields} Measuring the phase profile of a field effect transistor with 3 nm lateral resolution at field of view of 200 nm.

  7. Lateral resolution testing of a novel developed confocal microscopic imaging system

    Science.gov (United States)

    Zhang, Xin; Zhang, Yunhai; Chang, Jian; Huang, Wei; Xue, Xiaojun; Xiao, Yun

    2015-10-01

    Laser scanning confocal microscope has been widely used in biology, medicine and material science owing to its advantages of high resolution and tomographic imaging. Based on a set of confirmatory experiments and system design, a novel confocal microscopic imaging system is developed. The system is composed of a conventional fluorescence microscope and a confocal scanning unit. In the scanning unit a laser beam coupling module provides four different wavelengths 405nm 488nm 561nm and 638nm which can excite a variety of dyes. The system works in spot-to-spot scanning mode with a two-dimensional galvanometer. A 50 microns pinhole is used to guarantee that stray light is blocked and only the fluorescence signal from the focal point can be received . The three-channel spectral splitter is used to perform fluorescence imaging at three different working wavelengths simultaneously. The rat kidney tissue slice is imaged using the developed confocal microscopic imaging system. Nucleues labeled by DAPI and kidney spherule curved pipe labeled by Alexa Fluor 488 can be imaged clearly and respectively, realizing the distinction between the different components of mouse kidney tissue. The three-dimensional tomographic imaging of mouse kidney tissue is reconstructed by several two-dimensional images obtained in different depths. At last the resolution of the confocal microscopic imaging system is tested quantitatively. The experimental result shows that the system can achieve lateral resolution priority to 230nm.

  8. Enhancement of fluorescence confocal scanning microscopy lateral resolution by use of structured illumination

    International Nuclear Information System (INIS)

    Kim, Taejoong; Gweon, DaeGab; Lee, Jun-Hee

    2009-01-01

    Confocal microscopy is an optical imaging technique used to reconstruct three-dimensional images without physical sectioning. As with other optical microscopes, the lateral resolution of the confocal microscope cannot surpass the diffraction limit. This paper presents a novel imaging system, structured illumination confocal scanning microscopy (SICSM), that uses structured illumination to improve the lateral resolution of the confocal microscope. The SICSM can easily be implemented by introducing a structured illumination generating optics to conventional line-scanning fluorescence confocal microscopy. In this paper, we report our analysis of the lateral and axial resolutions of the SICSM by use of mathematical imaging theory. Numerical simulation results show that the lateral resolution of the SICSM is 1.43-fold better than that of the confocal microscope. In the axial direction, however, the resolution of the SICSM is ∼15% poorer than that of the confocal microscope. This deterioration arises because of a decrease in the axial cut-off frequency caused by the process of generating structured illumination. We propose the use of imaging conditions under which a compromise between the axial and lateral resolutions is chosen. Finally, we show simulated images of diversely shaped test objects to demonstrate the lateral and axial resolution performance of the SICSM

  9. ROV seafloor surveys combining 5-cm lateral resolution multibeam bathymetry with color stereo photographic imagery

    Science.gov (United States)

    Caress, D. W.; Hobson, B.; Thomas, H. J.; Henthorn, R.; Martin, E. J.; Bird, L.; Rock, S. M.; Risi, M.; Padial, J. A.

    2013-12-01

    at three sites in the deep Monterey Canyon axis. The surveys lines were spaced 1.5-m and were flown at speeds of 0.1-0.2-m/s while the sonars pinged at 3 Hz and the cameras operated at 0.5 Hz. All three low-altitude surveys are at ~2850 m depth and lie within the 1-m lateral resolution bathymetry of a 2009, 50-m altitude MBARI Mapping AUV survey. Site 1 has the greatest topography, being centered on a 15 m diameter, 7 m high flat boulder surrounded by an 80 m diameter, 6 m deep scour pit. Site 2 is located within a field of ~3-m high apparent sediment waves with ~80-m wavelengths. Site 0 is flat and includes chemosynthetic clam communities. At a 2 m altitude, the multibeam bathymetry swath is more than 7 m wide and the camera images are 4 m wide. Following navigation adjustment to match features in overlapping bathymetry swaths, we achieve 5-cm lateral resolution topography overlain with ~1-mm scale photographic imagery.

  10. XPS and STM study of the growth and structure of passive films in high temperature water on a nickel-base alloy

    Energy Technology Data Exchange (ETDEWEB)

    Machet, A.; Galtayries, A.; Zanna, S.; Klein, L.; Maurice, V.; Jolivet, P.; Foucault, M.; Combrade, P.; Scott, P.; Marcus, P

    2004-09-15

    The early stages of passivation in high temperature water of a nickel-chromium-iron alloy (Alloy 600) have been investigated by X-ray Photoelectron Spectroscopy (XPS) and Scanning Tunneling Microscopy (STM). The samples (polycrystal Ni-16Cr-9Fe (wt. %) and single crystal Ni-17Cr-7Fe (1 1 1)) have been exposed for short time periods (0.4-8.2 min) to high temperature (325 deg. C) and high pressure water, under controlled hydrogen pressure, in a microautoclave designed to transfer the samples from and to the XPS spectrometer without air exposure. In the early stages of oxidation of the alloy (0.4-4 min), an ultra-thin oxide layer (about 1 nm) is formed, which consists of chromium oxide (Cr{sub 2}O{sub 3}), according to the Cr 2p{sub 3/2} core level spectrum. An outer layer of Cr(OH){sub 3} with a very small amount of Ni(OH){sub 2} is also revealed by the Cr 2p{sub 3/2}, Ni 2p{sub 3/2}, and O 1s core level spectra. At this early stage, there is a temporary blocking of the growth of Cr{sub 2}O{sub 3}. For longer exposures (4-8 min), the Cr{sub 2}O{sub 3} inner layer becomes thicker, at the expense of the outer Cr(OH){sub 3} layer. This implies the transport of Cr and Ni through the oxide layer, and release of Ni{sup 2+} in the solution. The structure of the ultra-thin oxide film formed on a single crystal Ni-17Cr-7Fe(1 1 1) alloy was analysed by STM in the constant current mode; STM images reveal that, in the early stages of oxidation, the oxide is crystalline, and the observed structure is consistent with the hexagonal structure of the oxygen sub-lattice in the basal plane (0 0 0 1) of {alpha}-Cr{sub 2}O{sub 3}.

  11. High resolution XPS of the S 2p core level region of the L-cysteine/gold interface

    International Nuclear Information System (INIS)

    Cavalleri, O; Gonella, G; Terreni, S; Vignolo, M; Pelori, P; Floreano, L; Morgante, A; Canepa, M; Rolandi, R

    2004-01-01

    L-cysteine self-assembled monolayers (SAMs) have been deposited on gold from the liquid and vapour phase. Synchrotron based high resolution x-ray photoemission spectroscopy has been used to characterize the sulfur chemical states at the SAM/gold interface. Results obtained from pristine and x-ray irradiated samples, prepared with both as-received and purified L-cysteine, are reported. Pristine samples prepared with purified cysteine are characterized by an intense, largely dominant S 2p state at a binding energy around 162 eV (2p 3/2 level) assigned to thiolates. A second doublet around 161 eV develops during irradiation. By comparison with the literature, this doublet is assigned to atomic sulfur present either as impurity or generated by S-C bond scission. Comparative measurements performed, under similar experimental conditions, on pristine 3-mercaptopropionic acid [HS(CH 2 ) 2 COOH] layers deposited from the liquid phase are also presented and discussed

  12. IMPROVING VERTICAL AND LATERAL RESOLUTION BY STRETCH-FREE, HORIZON-ORIENTED IMAGING

    Directory of Open Access Journals (Sweden)

    Pérez Gabriel

    2006-12-01

    Full Text Available The pre-stack Kirchhoff migration is implemented for delivering wavelet stretch-free imaged data, if the migration is (ideally limited to the wavelet corresponding to a target horizon. Avoiding wavelet stretch provides long-offset imaged data, far beyond what is reached in conventional migration and results in images from the target with improved vertical and lateral resolution and angular illumination. Increasing the range of imaged offsets also increases the sensitivity to event-crossing, velocity errors and anisotropy. These issues must be addressed to fully achieve the greatest potential of this technique. These ideas are further illustrated with a land survey seismic data application in Texas, U.S.

  13. A novel method for enhancing the lateral resolution and image SNR in confocal microscopy

    Science.gov (United States)

    Chen, Youhua; Zhu, Dazhao; Fang, Yue; Kuang, Cuifang; Liu, Xu

    2017-12-01

    There is always a tradeoff between the resolution and the signal-to-noise ratio (SNR) in confocal microscopy. In particular, the pinhole size is very important for maintaining a balance between them. In this paper, we propose a method for improving the lateral resolution and image SNR in confocal microscopy without making any changes to the hardware. By using the fluorescence emission difference (FED) approach, we divide the images acquired by different pinhole sizes into one image acquired by the central pinhole and several images acquired by ring-shaped pinholes. Then, they are added together with the deconvolution method. Simulation and experimental results for fluorescent particles and cells show that our method can achieve a far better resolution than a large pinhole and a higher SNR than a small pinhole. Moreover, our method can improve the performance of classic confocal laser scanning microscopy (CLSM) to a certain extent, especially CLSM with a continuously variable pinhole.

  14. Characterization of the surface of Fe–19Mn–18Cr–C–N during heat treatment in a high vacuum — An XPS study

    International Nuclear Information System (INIS)

    Zumsande, K.; Weddeling, A.; Hryha, E.; Huth, S.; Nyborg, L.; Weber, S.; Krasokha, N.; Theisen, W.

    2012-01-01

    Nitrogen-containing CrMn austenitic stainless steels offer evident benefits compared to CrNi-based grades. The production of high-quality parts by means of powder metallurgy could be an appropriate alternative to the standard molding process leading to improved properties. The powder metallurgical production of CrMn austenitic steel is challenging on account of the high oxygen affinity of Mn and Cr. Oxides hinder the densification processes and may lower the performance of the sintered part if they remain in the steel after sintering. Thus, in evaluating the sinterability of the steel Fe–19Mn–18Cr–C–N, characterization of the surface is of great interest. In this study, comprehensive investigations by means of X-ray photoelectron spectroscopy and scanning electron microscopy combined with energy dispersive X-ray spectroscopy were performed to characterize the surface during heat treatment in a high vacuum. The results show a shift of oxidation up to 600 °C, meaning transfer of oxygen from the iron oxide layer to Mn-based particulate oxides, followed by progressive reduction and transformation of the Mn oxides into stable Si-containing oxides at elevated temperatures. Mass loss caused by Mn evaporation was observed accompanied by Mn oxide decomposition starting at 700 °C. - Highlights: ► Surface characterization by means of XPS, SEM, and EDX analyses. ► Heat treatment of a high CrMn powder. ► Transfer of oxygen from the iron oxide layer to manganese-based particulate oxides. ► Progressive reduction of Mn oxides. ► Transformation of the Mn oxides into stable Si-containing oxides.

  15. Imaging XPS - a new technique

    International Nuclear Information System (INIS)

    Gurker, N.; Ebel, M.F.; Ebel, H.

    1983-01-01

    XPS imaging promises to be a powerful analytic tool because it enables specific information on both elements and bonding to be recorded on a two-dimensional distribution map. As far as the authors are aware, the only scanning XPS method to date which has been found to be practical is essentially a scanned-particle-beam method, like scanning AES, and it is only applicable to thin film specimens. This paper provides the basic ideas of a new imaging XPS technique based on a quite different concept. It will be applicable to any kind of specimen that can be analysed in a conventional XPS system. It makes use of the dispersion properties of a spherical condenser-type spectrometer and applies a two-dimensional electron detection device for decoding the energy and emission position of an analysed photoelectron. Experimental arrangement and theory of operation are presented. (author)

  16. Design concept of the high-resolution end-station PEAXIS at BESSY II: Wide-Q-range RIXS and XPS measurements on solids, solutions, and interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Lieutenant, Klaus, E-mail: klaus.lieutenant@helmholtz-berlin.de [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Hofmann, Tommy, E-mail: tommy.hofmann@helmholtz-berlin.de [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Schulz, Christian, E-mail: schulz-c@helmholtz-berlin.de [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Yablonskikh, Mikhail V., E-mail: mikhail.yablonskikh@helmholtz-berlin.de [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Department of Physics, Freie Universität Berlin, Arnimallee 14, 14195 Berlin (Germany); Habicht, Klaus, E-mail: habicht@helmholtz-berlin.de [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Aziz, Emad F., E-mail: emad.aziz@helmholtz-berlin.de [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Department of Physics, Freie Universität Berlin, Arnimallee 14, 14195 Berlin (Germany); Institute for Molecular Science, Myodaiji 444-8585, Okazaki (Japan)

    2016-07-15

    Highlights: • Continuous rotation of the RIXS arm allowing truly Q-dependent measurements. • A systematic way to assess all RIXS spectrometer parameters using a figure of merit. • An analytical calculation of the energy dependent settings of a RIXS spectrometer. • Robustness analysis of spectrometer parameters for tolerances in engineering design. - Abstract: The design of a soft X-ray end-station for the Berlin Electron Synchrotron BESSY II is presented. It will be used for Resonant Inelastic X-ray Scattering (RIXS) and Angle-dependent X-ray Photoelectron Spectroscopy (AdXPS) studies for energy material science. In RIXS-mode the instrument operates with two spherical Variable Line Space (VLS) gratings for energy resolving measurements in two overlapping energy ranges from 200 to 1200 eV. The end-station will allow measurements of solid samples, solutions and interfaces in a wide range of experimental conditions with high energy resolution covering a large Q-range realized by a continuous rotation of the RIXS detector arm by 120°. Besides the description of this end-station, a systematic way is shown for the design of a RIXS instrument assessing the grating parameters based on existing theories and for the calculation of optimal instrument settings as a function of photon energy. Different grating inclinations, line densities, groove shapes and RIXS instrument lengths were investigated. Possible parameter combinations were calculated analytically and the resulting instrument performance was determined by ray-tracing simulations using the simulation package RAY. The performance of the RIXS instrument was evaluated by choosing the product of the intensity at the detector and the square of the resolving power as figure of merit to optimize the spectrometer. The robustness of the optimized parameters has been checked in order to define tolerance parameters for the engineering design of the spectrometer.

  17. The adsorption of NO on an oxygen pre-covered Pt(1 1 1) surface: in situ high-resolution XPS combined with molecular beam studies

    Science.gov (United States)

    Zhu, J. F.; Kinne, M.; Fuhrmann, T.; Tränkenschuh, B.; Denecke, R.; Steinrück, H.-P.

    2003-12-01

    Adsorption of NO on a Pt(1 1 1) surface pre-covered with a p(2 × 2) atomic oxygen layer has been studied in situ by high-resolution X-ray photoelectron spectroscopy and temperature-programmed XPS using third-generation synchrotron radiation at BESSY II, Berlin, combined with molecular beam techniques and ex situ by low energy electron diffraction and temperature-programmed desorption. O 1s XP spectra reveal that an ordered p(2 × 2)-O layer dramatically changes the adsorption behavior of NO as compared to the clean surface. The atomic oxygen occupies fcc hollow sites, and therefore blocks NO adsorption on these sites, which are energetically preferred on clean Pt(1 1 1). As a consequence, NO populates on-top sites at low coverage. At 110 K for higher coverages, NO can additionally adsorb on hcp hollow sites, thereby inducing a shift of the O 1s binding energy of atomic oxygen towards lower energies by about 0.25 eV. The bond strength of the hcp hollow NO species to the substrate is weakened by the presence of atomic oxygen. A sharp p(2 × 2) LEED pattern is observed for NO adsorption on the oxygen pre-covered surface, up to saturation coverage. The total saturation coverage of NO on Pt(1 1 1) pre-covered with varying amounts of oxygen (below 0.25 ML) decreases linearly with the coverage of oxygen. The initial sticking coefficient of NO is reduced from 0.96 on clean Pt(1 1 1) to 0.88 on a p(2 × 2) oxygen pre-covered surface.

  18. MOUTSINGA.xps

    African Journals Online (AJOL)

    HP Pro 2000

    L'étude vise à évaluer le régime alimentaire des poissons-chats du bassin de la rivière Léfini selon les ... 3 espèces de poissons, en fonction des saisons, le coefficient de condition, le pourcentage d'occurrence, ... subsidence, the food regime of C. ornatus, varied more than in periods of rise in the water level, with high.

  19. Torsional resonance mode magnetic force microscopy: enabling higher lateral resolution magnetic imaging without topography-related effects

    International Nuclear Information System (INIS)

    Kaidatzis, A; García-Martín, J M

    2013-01-01

    We present experimental work that reveals the benefits of performing magnetic force microscopy measurements employing the torsional resonance mode of cantilever oscillation. This approach provides two clear advantages: the ability of performing magnetic imaging without topography-related interference and the significant lateral resolution improvement (approximately 15%). We believe that this work demonstrates a significant improvement to a versatile magnetic imaging technique widely used in academia and in industry. (paper)

  20. XPS investigations of tribofilms formed on CrN coatings

    Energy Technology Data Exchange (ETDEWEB)

    Mandrino, Djordje, E-mail: djordje.mandrino@imt.si; Podgornik, Bojan

    2017-02-28

    Highlights: • Formation of tribofilms from lubricant additives on CrN surfaces during tribological contact confirmed by XPS. • Chemistry & chemical state of tribofilms obtained by XPS. • Thin sulphate film forms at the top of sulphide tribofilm. • Final type of sulphide in tribolayer depends on additive chemistry and testing temperature. - Abstract: Action of lubrication additives in the case of uncoated steel surfaces, including the type and mechanism of tribofilm formation is well known and understood. However, contact type of tribofilms which might form under the tribological contact between CrN coated surfaces, remains more or less unexplored. The aim of this investigation was to study the type of tribofilms formed on the CrN coated steel samples subjected to lubricated reciprocating sliding contact under different contact conditions Contact surface and tribofilms formed were studied by X-ray Photoelectron Spectroscopy (XPS). Sample surfaces were first imaged by Scanning Electron Microscopy (SEM) to determine areas of tribofilm formation as well as areas not affected by tribological contact. In these areas survey and high resolution (HR) XPS measurements were performed to obtain information about surface chemistry and oxidation states of the constituent elements. It was found that differences between different samples, observed by the XPS measurements, may reflect differences in chemistry of tribofilms formed under different contact conditions.

  1. XPS study of palladium sensitized nano porous silicon thin film

    Indian Academy of Sciences (India)

    Keywords. Porous silicon; passivation; palladium; oxidation; XPS. Abstract. Nano porous silicon (PS) was formed on -type monocrystalline silicon of 2–5 cm resistivity and (100) orientation by electrochemical anodization method using HF and ethanol as the electrolytes. High density of surface states, arising due to its ...

  2. Introduction to x-ray photoelectron spectroscopy (XPS)

    International Nuclear Information System (INIS)

    Liesegang, J.; Pigram, P.J.

    1999-01-01

    Full text: XPS is one of several important surface analytical tools. Developed in Sweden in the 1960s, it was originally named by Kai Siegbahn as Electron Spectroscopy for Chemical Analysis or ESCA; and although it is the best method for non-invasively determining the elemental composition of the first 10 nm of any surface, modern XPS systems are capable of much more than elemental chemical analysis. High resolution photoelectron energy analysis (c. 0.2 eV) now permits easy identification of chemical state as well as concentration; angular variation of detection and depth profiling allow quantitative analysis as a function of depth below a sample surface; energy loss mechanisms may be studied; Auger peaks can be measured in an XPS system; and developments in the area of photoelectron imaging allow high resolution (c. 7 μm) mapping of the distribution of elements and their chemical states to be determined spatially on non-homogeneous surfaces. The workshop sessions will outline the link between the physics and chemistry of surfaces and the process of photoemission. The presentation will illustrate the features and capabilities of a newly acquired Kratos (UK) Axis Ultra XPS and Imaging System recently installed in the Centre for Materials and Surface Science at La Trobe University, and its capabilities regarding the foregoing issues. The first part of the presentation will outline the basics of XPS and the second part will illustrate its usefulness, and in particular, will illustrate the power of the instrumentation through the presentation of several applications of both fundamental and industrial significance. Copyright (1999) Australian X-ray Analytical Association Inc

  3. Structural, photoluminescence and XPS properties of Tm3þ ions in ZnO nanostructures

    CSIR Research Space (South Africa)

    Kabongo, GL

    2017-07-01

    Full Text Available of photoluminescence (PL) spectroscopy. Finally, Tm 4d core level was detected in ZnO: 0.5 mol% Tm(sup3+) sample from high resolution X-Ray Photoelectron Spectroscopy (XPS) scan....

  4. On calculating intensity from XPS spectra

    International Nuclear Information System (INIS)

    Vegh, Janos

    2006-01-01

    The intensity calculation is the basis for all quantitative applications of electron spectroscopy. Unfortunately, some misinterpreted terms are used and correctly interpreted terms are misused in the overwhelming majority of publications in XPS, including most textbooks as well as accepted and proposed standards. Due to this mistake the number of the detected electrons is given as having dimension of energy (?) and also the formulas for calculating the peak area and its standard deviation are wrong. Since in all other spectroscopic fields the number of the detected particles is dimensionless, continuing this practice leads to isolating XPS from both other measurement sciences and theory, because the measured total intensity in XPS is simply not comparable to the ones derived with other spectroscopic methods or theoretically. Therefore, the basic measuring processes and terms are critically reviewed and their physically correct interpretation is given. This interpretation reveals that the error is hidden in the incorrect interpretation of both the measurement process and the measured quantity. It is shown that through using the correct interpretation both the dimensions of the intensity calculated from electron spectroscopic measurements as well as the formulas related to the intensity and its standard deviation will agree with all other spectroscopic fields

  5. The use of XPS and i.r. spectroscopy in zinc mineral flotation studies

    International Nuclear Information System (INIS)

    Garbassi, F.; Morabini, A.; Cozza, C.

    1985-01-01

    In this work, XPS (X-ray photoelectron spectroscopy) is applied to the study of the interaction of dodecylamine acetate with smithsonite ZnCo 3 , in relation with the problem of flotation of the mineral. This study confirms that, in spite of ultra-high conditions during analysis XPS is a technique offering a very valuable contribution to the elucidation of mineral flotation problems

  6. XPS, AES and laser raman spectroscopy: A fingerprint for a materials surface characterisation

    International Nuclear Information System (INIS)

    Zaidi Embong

    2011-01-01

    This review briefly describes some of the techniques available for analysing surfaces and illustrates their usefulness with a few examples such as a metal and alloy. In particular, Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) and laser Raman spectroscopy are all described as advanced surface analytical techniques. In analysing a surface, AES and XPS would normally be considered first, with AES being applied where high spatial resolution is required and XPS where chemical state information is needed. Laser Raman spectroscopy is useful for determining molecular bonding. A combination of XPS, AES and Laser Raman spectroscopy can give quantitative analysis from the top few atomic layers with a lateral spatial resolution of < 10 nm. (author)

  7. XPS - an essential tool in biomaterial research

    Energy Technology Data Exchange (ETDEWEB)

    StJohn, H.A.W.; Greisser, H.J. [Commonwealth Scientific and Industrial Research Organization (CSIRO), Clayton, VIC (Australia). Molecular Science

    1999-12-01

    Full text: Increased life expectancy has markedly enhanced the need for biomedical devices to combat life-threatening conditions (e.g., pacemakers, artificial blood vessels) or improve the quality of life (e.g., intraocular lenses, artificial ligaments, contact lenses). While the biomedical device industry has delivered remarkable benefits, many existing and emerging needs and applications are not adequately met with existing synthetic materials. Depending on the application, a biomaterial needs to meet a number of requirements to be `biocompatible`, such as appropriate mechanical properties, transparency, resistance to enzymatic degradation, and appropriate biological responses by the host environment. Surface science and surface analysis plays a key role in understanding and optimizing the molecular interfacial interactions between synthetic materials surfaces and biological media which lead to biological responses to implants. Many biological molecules such as proteins and lipids have surfactant activity and respond to interfaces on contact. Thus, an important part of achieving `biocompatibility` is to produce an appropriate surface chemical composition that avoids undesirable biological consequences triggered by biological molecules recognizing a `foreign` material interface. XPS surface analysis has proved uniquely suitable for studying several aspects of biomaterials. In order to interpret biological responses in terms of surface chemistry, it is essential that the surface be well characterized. However, for polymers this can be quite a challenge due to the inherent mobility of polymer chains. For instance, polyurethanes present a surface chemistry that differs from the `bulk` chemistry. It is often desirable to utilize a bulk material with desirable bulk properties and improve its biocompatibility by the application of a surface modification or a thin coating. XPS has been used to verify the intended coating chemistry and the uniformity of thin coatings. On

  8. XPS - an essential tool in biomaterial research

    International Nuclear Information System (INIS)

    StJohn, H.A.W.; Greisser, H.J.

    1999-01-01

    Full text: Increased life expectancy has markedly enhanced the need for biomedical devices to combat life-threatening conditions (e.g., pacemakers, artificial blood vessels) or improve the quality of life (e.g., intraocular lenses, artificial ligaments, contact lenses). While the biomedical device industry has delivered remarkable benefits, many existing and emerging needs and applications are not adequately met with existing synthetic materials. Depending on the application, a biomaterial needs to meet a number of requirements to be 'biocompatible', such as appropriate mechanical properties, transparency, resistance to enzymatic degradation, and appropriate biological responses by the host environment. Surface science and surface analysis plays a key role in understanding and optimizing the molecular interfacial interactions between synthetic materials surfaces and biological media which lead to biological responses to implants. Many biological molecules such as proteins and lipids have surfactant activity and respond to interfaces on contact. Thus, an important part of achieving 'biocompatibility' is to produce an appropriate surface chemical composition that avoids undesirable biological consequences triggered by biological molecules recognizing a 'foreign' material interface. XPS surface analysis has proved uniquely suitable for studying several aspects of biomaterials. In order to interpret biological responses in terms of surface chemistry, it is essential that the surface be well characterized. However, for polymers this can be quite a challenge due to the inherent mobility of polymer chains. For instance, polyurethanes present a surface chemistry that differs from the 'bulk' chemistry. It is often desirable to utilize a bulk material with desirable bulk properties and improve its biocompatibility by the application of a surface modification or a thin coating. XPS has been used to verify the intended coating chemistry and the uniformity of thin coatings. On

  9. Applications Performance on NAS Intel Paragon XP/S - 15#

    Science.gov (United States)

    Saini, Subhash; Simon, Horst D.; Copper, D. M. (Technical Monitor)

    1994-01-01

    The Numerical Aerodynamic Simulation (NAS) Systems Division received an Intel Touchstone Sigma prototype model Paragon XP/S- 15 in February, 1993. The i860 XP microprocessor with an integrated floating point unit and operating in dual -instruction mode gives peak performance of 75 million floating point operations (NIFLOPS) per second for 64 bit floating point arithmetic. It is used in the Paragon XP/S-15 which has been installed at NAS, NASA Ames Research Center. The NAS Paragon has 208 nodes and its peak performance is 15.6 GFLOPS. Here, we will report on early experience using the Paragon XP/S- 15. We have tested its performance using both kernels and applications of interest to NAS. We have measured the performance of BLAS 1, 2 and 3 both assembly-coded and Fortran coded on NAS Paragon XP/S- 15. Furthermore, we have investigated the performance of a single node one-dimensional FFT, a distributed two-dimensional FFT and a distributed three-dimensional FFT Finally, we measured the performance of NAS Parallel Benchmarks (NPB) on the Paragon and compare it with the performance obtained on other highly parallel machines, such as CM-5, CRAY T3D, IBM SP I, etc. In particular, we investigated the following issues, which can strongly affect the performance of the Paragon: a. Impact of the operating system: Intel currently uses as a default an operating system OSF/1 AD from the Open Software Foundation. The paging of Open Software Foundation (OSF) server at 22 MB to make more memory available for the application degrades the performance. We found that when the limit of 26 NIB per node out of 32 MB available is reached, the application is paged out of main memory using virtual memory. When the application starts paging, the performance is considerably reduced. We found that dynamic memory allocation can help applications performance under certain circumstances. b. Impact of data cache on the i860/XP: We measured the performance of the BLAS both assembly coded and Fortran

  10. Tl Cuprate Superconductors Studied by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Vasquez, R. P. [Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA 91109-8099 (United States); Siegal, M. P. [Sandia National Laboratories, Albuquerque, NM 87185-1421 (United States); Overmyer, D. L. [Sandia National Laboratories, Albuquerque, NM 87185-1421 (United States); Ren, Z. F. [Department of Chemistry, State University of New York, Buffalo, NY 14260-3000 (United States); Lao, J. Y. [Department of Chemistry, State University of New York, Buffalo, NY 14260-3000 (United States); Wang, J. H. [Department of Chemistry, State University of New York, Buffalo, NY 14260-3000 (United States)

    1999-07-01

    XPS measurements on epitaxial thin films of the Tl cuprate superconductors Tl2Ba2CaCu2O8, Tl2Ba2Ca2Cu3O10, and Tl0.78Bi0.22Ba0.4Sr1.6Ca2Cu3O9-{delta} are presented. These data, together with previous measurements in this lab on Tl2Ba2CuO6-{delta} and TlBa2CaCu2O7-{delta}, comprise a comprehensive data set for comparison of Tl cuprates in which the number of Tl-O and Cu-O layers, and hence the chemical and electronic properties, vary. (c) 2000 American Vacuum Society.

  11. Tl Cuprate Superconductors Studied by XPS

    International Nuclear Information System (INIS)

    Vasquez, R. P.; Siegal, M. P.; Overmyer, D. L.; Ren, Z. F.; Lao, J. Y.; Wang, J. H.

    1999-01-01

    XPS measurements on epitaxial thin films of the Tl cuprate superconductors Tl2Ba2CaCu2O8, Tl2Ba2Ca2Cu3O10, and Tl0.78Bi0.22Ba0.4Sr1.6Ca2Cu3O9-δ are presented. These data, together with previous measurements in this lab on Tl2Ba2CuO6-δ and TlBa2CaCu2O7-δ, comprise a comprehensive data set for comparison of Tl cuprates in which the number of Tl-O and Cu-O layers, and hence the chemical and electronic properties, vary. (c) 2000 American Vacuum Society

  12. XPS analysis of boron doped heterofullerenes

    Energy Technology Data Exchange (ETDEWEB)

    Schnyder, B; Koetz, R [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Muhr, H J; Nesper, R [ETH Zurich, Zurich (Switzerland)

    1997-06-01

    Boron heterofullerenes were generated through arc-evaporation of doped graphite rods in a helium atmosphere. According to mass spectrometric analysis only mono-substituted fullerenes like C{sub 59}B, C{sub 69}B and higher homologues together with a large fraction of higher undoped fullerenes were extracted and enriched when pyridine was used as the solvent. XPS analysis of the extracts indicated the presence of two boron species with significantly different binding energies. One peak was assigned to borid acid. The second one corresponds to boron in the fullerene cage, which is mainly C{sub 59}B, according to the mass spectrum. This boron is in a somewhat higher oxidation state than that of ordinary boron-carbon compounds. The reported synthesis and extraction procedure opens a viable route for production of macroscopic amounts of these compounds. (author) 2 figs., 1 tab., 7 refs.

  13. Secondary electron measurement and XPS characterization of NEG coatings

    International Nuclear Information System (INIS)

    Sharma, R. K.; Sinha, Atul K.; Gupta, Nidhi; Nuwad, J.; Jagannath,; Gadkari, S. C.; Singh, M. R.; Gupta, S. K.

    2014-01-01

    Ternary alloy coatings of IVB and VB materials provide many of benefits over traditional material surfaces such as creation of extreme high vacuum(XHV), lower secondary electron yield(SEY), low photon desorption coefficient. XHV (pressure −10 mbar) is very useful to the study of surfaces of the material in as it is form, high energy particle accelerators(LHC, Photon Factories), synchrotrons (ESRF, Ellectra) etc.. Low secondary electron yield leads to very low multi-pacting utilizes to increase beam life time. In this paper preparation of the coatings and a study of secondary electron yield measurement after heating at different temperatures has been shown also results of their surface characterization based on shift in binding energy has been produced using the surface techniques XPS. Stoichiometry of the film was measured by Energy dispersive x-ray analysis (EDX)

  14. XPS and bioactivity study of the bisphosphonate pamidronate adsorbed onto plasma sprayed hydroxyapatite coatings

    International Nuclear Information System (INIS)

    McLeod, Kate; Kumar, Sunil; Smart, Roger St.C.; Dutta, Naba; Voelcker, Nicolas H.; Anderson, Gail I.; Sekel, Ron

    2006-01-01

    This paper reports the use of X-ray photoelectron spectroscopy (XPS) to investigate bisphosphonate (BP) adsorption onto plasma sprayed hydroxyapatite (HA) coatings commonly used for orthopaedic implants. BPs exhibit high binding affinity for the calcium present in HA and hence can be adsorbed onto HA-coated implants to exploit their beneficial properties for improved bone growth at the implant interface. A rigorous XPS analysis of pamidronate, a commonly used nitrogenous BP, adsorbed onto plasma sprayed HA-coated cobalt-chromium substrates has been carried out, aimed at: (a) confirming the adsorption of this BP onto HA; (b) studying the BP diffusion profile in the HA coating by employing the technique of XPS depth profiling; (c) confirming the bioactivity of the adsorbed BP. XPS spectra of plasma sprayed HA-coated discs exposed to a 10 mM aqueous BP solution (pamidronate) for periods of 1, 2 and 24 h showed nitrogen and phosphorous photoelectron signals corresponding to the BP, confirming its adsorption onto the HA substrate. XPS depth profiling of the 2 h BP-exposed HA discs showed penetration of the BP into the HA matrix to depths of at least 260 nm. The bioactivity of the adsorbed BP was confirmed by the observed inhibition of osteoclast (bone resorbing) cell activity. In comparison to the HA sample, the HA sample with adsorbed BP exhibited a 25-fold decrease in primary osteoclast cells

  15. XPS characterization of surface and interfacial structure of sputtered TiNi films on Si substrate

    International Nuclear Information System (INIS)

    Fu Yongqing; Du Hejun; Zhang, Sam; Huang Weimin

    2005-01-01

    TiNi films were prepared by co-sputtering TiNi and Ti targets. X-ray photoelectron spectroscopy (XPS) was employed to study surface chemistry of the films and interfacial structure of Si/TiNi system. Exposure of the TiNi film to the ambient atmosphere (23 deg. C and 80% relatively humidity) facilitated quick adsorption of oxygen and carbon on the surface. With time, carbon and oxygen content increased drastically at the surface, while oxygen diffused further into the layer. After a year, carbon content at the surface became as high as 65.57% and Ni dropped below the detection limit of XPS. Depth profiling revealed that significant inter-diffusion occurred between TiNi film and Si substrate with a layer of 90-100 nm. The detailed bond changes of different elements with depth were obtained using XPS and the formation of titanium silicides at the interface were identified

  16. XPS studies of ceramics with pyrochlore structure for radioactive wastes disposal

    International Nuclear Information System (INIS)

    Teterin, Yu.A.; Vukchevich, L.; Ivanov, K.E.; Utkin, I.O; Teterin, A. Yu.; Maslakov, K.I.; Yudintseva, T.S.; Yudintsev, S.V.; Stefanovsky, S.V.; Lapina, M.I. . E-mail address of corresponding author: vukas@rc.pmf.cg.ac.yu; Vukchevich, L.)

    2005-01-01

    X-ray photoelectron spectroscopy (XPS) study of ceramics CaThSn 2 O 7 and CaThZr 2 O 7 with pyrochlore structure used as matrixes for the disposal of long lived high level radioactive wastes was done. On the basis of the XPS parameters of the core and outer electrons in the binding energy range 0 - 1000 eV the oxidation states of the included metals were determined, quantitative elemental and ionic analysis was carried out and a conclusion on the monophaseness of the studied samples was drawn. The obtained data agree with the X-ray diffraction and scanning electron microscopy results. (author)

  17. Quantification of the toxic hexavalent chromium content in an organic matrix by X-ray photoelectron spectroscopy (XPS) and ultra-low-angle microtomy (ULAM)

    Energy Technology Data Exchange (ETDEWEB)

    Greunz, Theresia, E-mail: theresia.greunz@jku.at [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterisation (CDL-MS-MACH), Center for Surface and Nanoanalytics (ZONA), Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Duchaczek, Hubert; Sagl, Raffaela [voestalpine Stahl GmbH, voestalpine-Straße 3, 4031 Linz (Austria); Duchoslav, Jiri; Steinberger, Roland [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterisation (CDL-MS-MACH), Center for Surface and Nanoanalytics (ZONA), Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Strauß, Bernhard [voestalpine Stahl GmbH, voestalpine-Straße 3, 4031 Linz (Austria); Stifter, David [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterisation (CDL-MS-MACH), Center for Surface and Nanoanalytics (ZONA), Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria)

    2017-02-28

    Highlights: • Common methods are not suitable for a reliable determination of Cr(VI) in organic coatings on steel. • Our proposed method is a combination of XPS and ultra-low-angle microtomy (ULAM). • The results allow referring to legal regulations of the Cr(VI) concentration. • For this method no accurate sample parameters are required. - Abstract: Cr(VI) is known for its corrosion inhibitive properties and is, despite legal regulations, still a potential candidate to be added to thin (1–3 μm) protective coatings applied on, e.g., electrical steel as used for transformers, etc. However, Cr(VI) is harmful to the environment and to the human health. Hence, a reliable quantification of it is of decisive interest. Commonly, an alkaline extraction with a photometric endpoint detection of Cr(VI) is used for such material systems. However, this procedure requires an accurate knowledge on sample parameters such as dry film thickness and coating density that are occasionally associated with significant experimental errors. We present a comprehensive study of a coating system with a defined Cr(VI) pigment concentration applied on electrical steel. X-ray photoelectron spectroscopy (XPS) was employed to resolve the elemental chromium concentration and the chemical state. Turning to the fact that XPS is extremely surface sensitive (<10 nm) and that the lowest commonly achievable lateral resolution is a number of times higher than the coating thickness (∼2 μm), a bulk analysis was achieved with XPS line scans on extended wedge-shaped tapers through the coating. For that purpose a special sample preparation step performed on an ultra-microtome was required prior to analysis. Since a temperature increase leads to a reduction of Cr(VI) we extend our method on samples, which were subjected to different curing temperatures. We show that our proposed approach now allows to determine the elemental and Cr(VI) concentration and distribution inside the coating.

  18. Effects of XPS operational parameters on investigated sample surfaces

    International Nuclear Information System (INIS)

    Mrad, O.; Ismail, I.

    2013-04-01

    In this work, we studied the effects of the operating conditions of the xray photoelectron spectroscopy analysis technique (XPS) on the investigated samples. Firstly, the performances of the whole system have been verified as well as the accuracy of the analysis. Afterwards, the problem of the analysis of insulating samples caused by the charge buildup on the surface has been studied. The use of low-energy electron beam (<100 eV) to compensate the surface charge has been applied. The effect of X-ray on the samples have been assessed and was found to be nondestructive within the analysis time. The effect of low- and high-energy electron beams on the sample surface have been investigated. Highenergy electrons were found to have destructive effect on organic samples. The sample heating procedure has been tested and its effect on the chemical stat of the surface was followed. Finally, the ion source was used to determine the elements distribution and the chemical stat of different depths of the sample. A method has been proposed to determine these depths (author).

  19. An XPS study on ruthenium compounds and catalysts

    International Nuclear Information System (INIS)

    Bianchi, C.L.; Ragaini, V.; Cattania, M.G.

    1991-01-01

    The binding energy (BE) of the relevant peaks of several ruthenium compounds have been measured with a monochromatic small spot XPS. The BE of the 3d 5/2 level of ruthenium is in the range 279.91-282.88 eV. The variation of BE is due either to the variation of the oxidation state or to the different counter-ion. A series of catalysts with varying amounts of ruthenium supported on alumina and prepared using different precursors was also analyzed. The presence of more ruthenium species other than the metal was observed. On the basis of the values previously obtained on unsupported compounds, the species with higher BE were assigned to oxides. On all the samples prepared from RuCl 3 , an additional peak at a very high BE (283.79 eV) has been observed. This peak is related to the presence of chlorine on the surface: it is suggested that it is related to a charge transfer interaction. The influence of this species on the CO reactivity in the Fischer-Tropsch reaction is discussed. (orig.)

  20. Geochemistry of the Cigar Lake uranium deposit: XPS studies

    International Nuclear Information System (INIS)

    Sunder, S.; Cramer, J.J.; Miller, N.H.

    1996-01-01

    Samples of uranium ore from the Cigar Lake deposit in northern Saskatchewan, Canada, were analyzed using XPS. High-resolution spectra were recorded for the strongest bands of the major elements (U 4f, C 1 s, O 1 s, Pb 4 f, S 2 p, Cu 2 p, Fe 2 p, and the valence region (0-20 eV)) to obtain chemical state information for these samples. In general, the U VI /U IV ratio was very low, i.e., much less than 0.5, the threshold for the oxidative dissolution of UO 2 . The low values of the U VI /U IV ratio observed for samples from the Cigar Lake deposit indicate thermodynamic stability of the uranium ore in the reduced aqueous environment. Similarities between the disposal vault envisaged in the Canadian Nuclear Fuel Waste Management Program and the Cigar Lake deposit suggest that, if geochemical conditions in the vault were to be similar to those in the deposit, the long-term dissolution of UO 2 fuel would be very minimal. (orig.)

  1. Theoretical modeling of the uranium 4f XPS for U(VI) and U(IV) oxides

    Energy Technology Data Exchange (ETDEWEB)

    Bagus, Paul S. [Department of Chemistry, University of North Texas, Denton, Texas 76203-5017 (United States); Nelin, Connie J. [Consulting and Services, 6008 Maury' s Trail, Austin, Texas 78730 (United States); Ilton, Eugene S. [Pacific Northwest National Laboratory, Richland, Washington 99352 (United States)

    2013-12-28

    A rigorous study is presented of the physical processes related to X-Ray photoelectron spectroscopy, XPS, in the 4f level of U oxides, which, as well as being of physical interest in themselves, are representative of XPS in heavy metal oxides. In particular, we present compelling evidence for a new view of the screening of core-holes that extends prior understandings. Our analysis of the screening focuses on the covalent mixing of high lying U and O orbitals as opposed to the, more common, use of orbitals that are nominally pure U or pure O. It is shown that this covalent mixing is quite different for the initial and final, core-hole, configurations and that this difference is directly related to the XPS satellite intensity. Furthermore, we show that the high-lying U d orbitals as well as the U(5f) orbital may both contribute to the core-hole screening, in contrast with previous work that has only considered screening through the U(5f) shell. The role of modifying the U-O interaction by changing the U-O distance has been investigated and an unexpected correlation between U-O distance and XPS satellite intensity has been discovered. The role of flourite and octahedral crystal structures for U(IV) oxides has been examined and relationships established between XPS features and the covalent interactions in the different structures. The physical views of XPS satellites as arising from shake processes or as arising from ligand to metal charge transfers are contrasted; our analysis provides strong support that shake processes give a more fundamental physical understanding than charge transfer. Our theoretical studies are based on rigorous, strictly ab initio determinations of the electronic structure of embedded cluster models of U oxides with formal U(VI) and U(IV) oxidation states. Our results provide a foundation that makes it possible to establish quantitative relationships between features of the XPS spectra and materials properties.

  2. Theoretical modeling of the uranium 4f XPS for U(VI) and U(IV) oxides

    Science.gov (United States)

    Bagus, Paul S.; Nelin, Connie J.; Ilton, Eugene S.

    2013-12-01

    A rigorous study is presented of the physical processes related to X-Ray photoelectron spectroscopy, XPS, in the 4f level of U oxides, which, as well as being of physical interest in themselves, are representative of XPS in heavy metal oxides. In particular, we present compelling evidence for a new view of the screening of core-holes that extends prior understandings. Our analysis of the screening focuses on the covalent mixing of high lying U and O orbitals as opposed to the, more common, use of orbitals that are nominally pure U or pure O. It is shown that this covalent mixing is quite different for the initial and final, core-hole, configurations and that this difference is directly related to the XPS satellite intensity. Furthermore, we show that the high-lying U d orbitals as well as the U(5f) orbital may both contribute to the core-hole screening, in contrast with previous work that has only considered screening through the U(5f) shell. The role of modifying the U-O interaction by changing the U-O distance has been investigated and an unexpected correlation between U-O distance and XPS satellite intensity has been discovered. The role of flourite and octahedral crystal structures for U(IV) oxides has been examined and relationships established between XPS features and the covalent interactions in the different structures. The physical views of XPS satellites as arising from shake processes or as arising from ligand to metal charge transfers are contrasted; our analysis provides strong support that shake processes give a more fundamental physical understanding than charge transfer. Our theoretical studies are based on rigorous, strictly ab initio determinations of the electronic structure of embedded cluster models of U oxides with formal U(VI) and U(IV) oxidation states. Our results provide a foundation that makes it possible to establish quantitative relationships between features of the XPS spectra and materials properties.

  3. XPS utilization in the characterization of glycerol based polyesters; Utilizacao de XPS na caracterizacao de poliesteres a base de glicerol

    Energy Technology Data Exchange (ETDEWEB)

    Brioude, M.M.; Miranda, C.S.; Pereira, R.; Ohara, L.; Bargiela, P.; Rocha, M.G.M.C.; Jose, N.M., E-mail: mgcr@ufba.b [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Inst. de Quimica

    2010-07-01

    X-ray photoelectron spectroscopy-XPS allows the determination of all elements of the periodical table, except hydrogen and helium, and is a very used technique for the polymers characterization, its spectra constitutes a 'fingerprint' of the material. Two samples of polymers were prepared from glycerol and fumaric acid and glycerol and terephthalic acid, with a molar ratio of 1:1 and 1:1.5. The general spectra show the presence of carbon and oxygen, the main components of the polymer. From the binding energies values of the C1s and O1s high resolution spectra it was possible to determine the carbon functional groups. Their concentration were determined and the presence of the aromatic carbon in the terephthalic polyesters was observed, and also similar proportions of aliphatic carbon and ester groups in the fumaric acid polyesters. For both polyesters, an amount of carboxyl group appears, indicating the terminal non-reacted groups. These results were confirmed qualitatively by FTIR. (author)

  4. Characterization of fossil remains using XRF, XPS and XAFS spectroscopies

    International Nuclear Information System (INIS)

    Zougrou, I M; Katsikini, M; Pinakidou, F; Paloura, E C; Brzhezinskaya, M; Papadopoulou, L; Vlachos, E; Tsoukala, E

    2016-01-01

    Synchrotron radiation micro-X-Ray Fluorescence (μ-XRF), X-ray photoelectron (XPS) and X-ray Absorption Fine Structure (XAFS) spectroscopies are applied for the study of paleontological findings. More specifically the costal plate of a gigantic terrestrial turtle Titanochelon bacharidisi and a fossilized coprolite of the cave spotted hyena Crocuta crocuta spelaea are studied. Ca L 2,3 -edge NEXAFS and Ca 2p XPS are applied for the identification and quantification of apatite and Ca containing minerals. XRF mapping and XAFS are employed for the study of the spatial distribution and speciation of the minerals related to the deposition environment. (paper)

  5. Pd adsorption on Si(1 1 3) surface: STM and XPS study

    International Nuclear Information System (INIS)

    Hara, Shinsuke; Yoshimura, Masamichi; Ueda, Kazuyuki

    2008-01-01

    Pd-induced surface structures on Si(1 1 3) have been studied by scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS). In the initial process of the Pd adsorption below 0.10 ML, Pd silicide (Pd 2 Si) clusters are observed to form randomly on the surface. By increasing the Pd coverage to 0.10 ML, the clusters cover the entire surface, and an amorphous layer is formed. After annealing the Si(1 1 3)-Pd surface at 600 deg. C, various types of islands and chain protrusions appears. The agglomeration, coalescence and crystallization of these islands are observed by using high temperature (HT-) STM. It is also found by XPS that the islands correspond to Pd 2 Si structure. On the basis of these results, evolution of Pd-induced structures at high temperatures is in detail discussed

  6. Synchrotron radiation as a source for quantitative XPS: advantages and consequences

    International Nuclear Information System (INIS)

    Rosseel, T.M.; Carlson, T.A.; Negri, R.E.; Beall, C.E.; Taylor, J.W.

    1986-01-01

    Synchrotron radiation (SR) has a variety of properties which make it an attractive source for quantitative x-ray photoelectron spectroscopy (XPS). Among the most significant are high intensity and tunability. In addition, the intensity of the dispersed radiation is comparable to laboratory line sources. Synchrotron radiation is also a clean source, i.e., it will not contaminate the sample, because it operates under ultra-high vacuum conditions. We have used these properties to demonstrate the advantages of SR as a source for quantitative XPS. We have also found several consequences associated with this source which can either limit its use or provide unique opportunities for analysis and research. Using the tunability of SR, we have measured the energy dependence of the 3p photoionization cross sections of Ti, Cr, and Mn from 50 to 150 eV above threshold at the University of Wisconsin's Tantalus electron-storage ring

  7. Study of room temperature Raman scattering and XPS, high temperature electrical and low temperature magnetic properties of Zn1−yLiyO (0.00 ≤y≤ 0.10) nanoparticles

    KAUST Repository

    Awan, Saif Ullah

    2015-10-15

    Multiferroics are potentially future materials in spintronics for memory and data storage applications. In this paper, a series of Li-doped nanoparticles were studied to investigate the effects of Li on the physical properties of the ZnO system. Analysis of structural micrographs and Raman spectra confirmed the wurtzite structure of doped samples. The vibrational modes of Zinc and oxygen atoms were labeled as E and E with an additional mode at 134 cm in the doped samples. We observed the presence of interstitial and substitutional Li defects from the deconvolution of Li 1s core level spectra using high resolution x-ray photoelectron spectroscopy. The approximated measured values (e.g., for y = 0.04 and 0.08 samples) for interstitial Li defects were 27% and 39%, and for substitutional Li defects were 73% and 61% respectively. For the y = 0.06 composition, dc resistivity was the highest, while the transition temperature (measured from dielectric loss) was the lowest. We observed a non-monotonic trend of saturation magnetization (obtained at 50 K) against the Li concentration. The compositions having the highest magnetic moment were those having higher interstitial Li defects and lower dc resistivity. Higher hole carrier concentrations and dielectric transition temperatures were correlated with the higher magnetization. Interstitial Li defects played a key role in stabilizing more cationic Zn vacancies. Hole carriers were the major cause of long-range ferromagnetic order in these nanoparticles.

  8. Study of room temperature Raman scattering and XPS, high temperature electrical and low temperature magnetic properties of Zn1−yLiyO (0.00 ≤y≤ 0.10) nanoparticles

    KAUST Repository

    Awan, Saif Ullah; Hasanain, S. K.; Mehmood, Zahid; Anjum, Dalaver H.; Shah, Saqlain A.; Aftab, M.; Abbas, Turab Ali

    2015-01-01

    Multiferroics are potentially future materials in spintronics for memory and data storage applications. In this paper, a series of Li-doped nanoparticles were studied to investigate the effects of Li on the physical properties of the ZnO system. Analysis of structural micrographs and Raman spectra confirmed the wurtzite structure of doped samples. The vibrational modes of Zinc and oxygen atoms were labeled as E and E with an additional mode at 134 cm in the doped samples. We observed the presence of interstitial and substitutional Li defects from the deconvolution of Li 1s core level spectra using high resolution x-ray photoelectron spectroscopy. The approximated measured values (e.g., for y = 0.04 and 0.08 samples) for interstitial Li defects were 27% and 39%, and for substitutional Li defects were 73% and 61% respectively. For the y = 0.06 composition, dc resistivity was the highest, while the transition temperature (measured from dielectric loss) was the lowest. We observed a non-monotonic trend of saturation magnetization (obtained at 50 K) against the Li concentration. The compositions having the highest magnetic moment were those having higher interstitial Li defects and lower dc resistivity. Higher hole carrier concentrations and dielectric transition temperatures were correlated with the higher magnetization. Interstitial Li defects played a key role in stabilizing more cationic Zn vacancies. Hole carriers were the major cause of long-range ferromagnetic order in these nanoparticles.

  9. XPS studies of the oxide formed on pure Ti

    International Nuclear Information System (INIS)

    Cremery, P.; David, D.; Beranger, G.; Oviedo, C.; Garcia, E.A.

    1980-01-01

    The XPS technique was used to study titanium samples oxidized at 200 ton of pure oxigen at different times and temperatures with the aim of producing variable oxide thicknesses. The thicknesses of different oxigen layers were determined by the nuclear reaction O 16 (d,p) O 17 *. (author) [pt

  10. Quantitative XPS analysis of thin iron-oxide films

    DEFF Research Database (Denmark)

    Graat, P.C.J.; Somers, Marcel A. J.

    1997-01-01

    Over the last decade Tougaard et al. (see e.g. Ref. 1) provided a formalism to calculate the contribution of inelastically scattered electrons to an XPS or AES spectrum. In that formalism it was assumed that the signal electrons move along straight lines to the surface. Recently, Werner et al. pr...

  11. XPS and angle resolved XPS, in the semiconductor industry: Characterization and metrology control of ultra-thin films

    International Nuclear Information System (INIS)

    Brundle, C.R.; Conti, Giuseppina; Mack, Paul

    2010-01-01

    This review discusses the development of X-ray photoelectron spectroscopy, XPS, used as a characterization and metrology method for ultra-thin films in the semiconductor wafer processing industry. After a brief explanation of how the relative roles of XPS and Auger electron spectroscopy, AES, have changed over the last 15 years or so in the semiconductor industry, we go into some detail as to what is implied by metrology, as opposed to characterization, for thin films in the industry, and then describe how XPS, and particularly angle resolved XPS, ARXPS, have been implemented as a metrology 'tool' for thickness, chemical composition, and non-destructive depth profiling, of transistor gate oxide material, a key requirement in front-end processing. We take a historical approach, dealing first with the early use for SiO 2 films on Si(1 0 0), then moving to silicon oxynitride, SiO x N y in detail, and finally and briefly HfO 2 -based material, which is used today in the most advanced devices (32 nm node).

  12. The hidden radiation chemistry in plasma modification and XPS analysis of polymer surfaces

    International Nuclear Information System (INIS)

    George, G.A.; Le, T.T.; Elms, F.M.; Wood, B.J.

    1996-01-01

    Full text: The surface modification of polymers using plasma treatments is being widely researched to achieve changes in the surface energetics and consequent wetting and reactivity for a range of applications. These include i) adhesion for polymer bonding and composite material fabrication and ii) biocompatibility of polymers when used as orthopedic implants, catheters and prosthetics. A low pressure rf plasma produces a variety of species from the introduced gas which may react with the surface of a hydrocarbon polymer, such as polyethylene. In the case of 0 2 and H 2 0, these species include oxygen atoms, singlet molecular oxygen and hydroxyl radicals, all of which may oxidise and, depending on their energy, ablate the polymer surface. In order to better understand the reactive species formed both in and downstream from a plasma and the relative contributions of oxidation and ablation, self-assembled monolayers of n-alkane thiols on gold are being used as well characterised substrates for quantitative X-ray photoelectron spectroscopy (XPS). The identification and quantification of oxidised carbon species on plasma treated polymers from broad, asymmetric XPS signals is difficult, so derivatisation is often used to enhance sensitivity and specificity. For example, trifluoroacetic anhydride (TFAA) selectively labels hydroxyl functionality. The surface analysis of a modified polymer surface may be confounded by high energy radiation chemistry which may occur during XPS analysis. Examples include scission of carbon-halogen bonds (as in TFM adducts), decarboxylation and main-chain polyene formation. The extent of free-radical chemistry occurring in polyethylene while undergoing XPS analysis may be seen by both ESR and FT-IR analysis

  13. Soft X-ray-induced decomposition of amino acids: An XPS, mass spectrometry, and NEXAFS study

    International Nuclear Information System (INIS)

    Zubavichus, Yan; Fuchs, Oliver; Weinhardt, Lothar; Heske, Clemens; Umbach, Eberhard; Denlinger, Jonathan D.; Grunze, Michael

    2003-01-01

    Decomposition of five amino acids, alanine, serine, cysteine, aspartic acid, and asparagine, under irradiation with soft X-rays (magnesium Ka X-ray source) in ultra-high vacuum was studied by means of X-ray photoelectron spectrometry (XPS) and mass spectrometry. A comparative analysis of changes in XPS line shapes, stoichiometry and residual gas composition indicates that the molecules decompose by several pathways. Dehydration, decarboxylation, decarbonylation,deamination and desulfurization of pristine molecules accompanied by desorption of H2, H2O, CO2, CO, NH3and H2S are observed with rates depending on the specific amino acid. NEXAFS spectra of cysteine at the carbon, oxygen and nitrogen K-shell and sulfur L2,3 edges complement the XPS and mass spectrometry data and show that the exposure of the sample to an intense soft X-ray synchrotron beam results in the formation of C-C and C-N double and triple bonds. Qualitatively, the amino acids studied can be arranged in the following ascending order of radiation stability:serine< alanine< aspartic acid< cysteine< asparagine

  14. Quantitative analysis of Si1-xGex alloy films by SIMS and XPS depth profiling using a reference material

    Science.gov (United States)

    Oh, Won Jin; Jang, Jong Shik; Lee, Youn Seoung; Kim, Ansoon; Kim, Kyung Joong

    2018-02-01

    Quantitative analysis methods of multi-element alloy films were compared. The atomic fractions of Si1-xGex alloy films were measured by depth profiling analysis with secondary ion mass spectrometry (SIMS) and X-ray Photoelectron Spectroscopy (XPS). Intensity-to-composition conversion factor (ICF) was used as a mean to convert the intensities to compositions instead of the relative sensitivity factors. The ICFs were determined from a reference Si1-xGex alloy film by the conventional method, average intensity (AI) method and total number counting (TNC) method. In the case of SIMS, although the atomic fractions measured by oxygen ion beams were not quantitative due to severe matrix effect, the results by cesium ion beam were very quantitative. The quantitative analysis results by SIMS using MCs2+ ions are comparable to the results by XPS. In the case of XPS, the measurement uncertainty was highly improved by the AI method and TNC method.

  15. Surface studies on uranium monocarbide using XPS and SIMS

    International Nuclear Information System (INIS)

    Asuvathraman, R.

    1995-01-01

    The air-exposed surfaces of sintered and arc-melted UC samples were examined by XPS and SIMS. XPS results indicate that the surface is covered with a very thin layer of UO 2 mixed with free carbon, which would have formed along with the oxide during the reaction between UC and oxygen or moisture. From the SIMS depth profile of oxygen, the thickness of the oxide layer is found to be approximately 10 nm. The SIMS oxygen images of the surface as a function of etching time reveal that the surface of UC consists of a top layer of adsorbed moisture/oxygen; this contamination layer is followed by a layer containing uranium oxide, uranium hydroxide and free carbon and then grain boundary oxide and finally bulk UC. The behaviour of sintered and arc-melted samples is similar. ((orig.))

  16. XPS studies of nitrogen doping niobium used for accelerator applications

    Science.gov (United States)

    Yang, Ziqin; Lu, Xiangyang; Tan, Weiwei; Zhao, Jifei; Yang, Deyu; Yang, Yujia; He, Yuan; Zhou, Kui

    2018-05-01

    Nitrogen doping study on niobium (Nb) samples used for the fabrication of superconducting radio frequency (SRF) cavities was carried out. The samples' surface treatment was attempted to replicate that of the Nb SRF cavities, which includes heavy electropolishing (EP), nitrogen doping and the subsequent EP with different amounts of material removal. The surface chemical composition of Nb samples with different post treatments has been studied by XPS. The chemical composition of Nb, O, C and N was presented before and after Gas Cluster Ion Beam (GCIB) etching. No signals of poorly superconducting nitrides NbNx was found on the surface of any doped Nb sample with the 2/6 recipe before GCIB etching. However, in the depth range greater than 30 nm, the content of N element is below the XPS detection precision scope even for the Nb sample directly after nitrogen doping treatment with the 2/6 recipe.

  17. XPS quantification of the hetero-junction interface energy

    International Nuclear Information System (INIS)

    Ma, Z.S.; Wang Yan; Huang, Y.L.; Zhou, Z.F.; Zhou, Y.C.; Zheng Weitao; Sun, Chang Q.

    2013-01-01

    Highlights: ► Quantum entrapment or polarization dictates the performance of dopant, impurity, interface, alloy and compounds. ► Interface bond energy, energy density, and atomic cohesive energy can be determined using XPS and our BOLS theory. ► Presents a new and reliable method for catalyst design and identification. ► Entrapment makes CuPd to be a p-type catalyst and polarization derives AgPd as an n-type catalyst. - Abstract: We present an approach for quantifying the heterogeneous interface bond energy using X-ray photoelectron spectroscopy (XPS). Firstly, from analyzing the XPS core-level shift of the elemental surfaces we obtained the energy levels of an isolated atom and their bulk shifts of the constituent elements for reference; then we measured the energy shifts of the specific energy levels upon interface alloy formation. Subtracting the referential spectrum from that collected from the alloy, we can distil the interface effect on the binding energy. Calibrated based on the energy levels and their bulk shifts derived from elemental surfaces, we can derive the bond energy, energy density, atomic cohesive energy, and free energy at the interface region. This approach has enabled us to clarify the dominance of quantum entrapment at CuPd interface and the dominance of polarization at AgPd and BeW interfaces, as the origin of interface energy change. Developed approach not only enhances the power of XPS but also enables the quantification of the interface energy at the atomic scale that has been an issue of long challenge.

  18. SORCE XPS Level 3 Solar Spectral Irradiance 6-Hour Means V010

    Data.gov (United States)

    National Aeronautics and Space Administration — The SORCE XUV Photometer System (XPS) Solar Spectral Irradiance (SSI) 6-Hour Data Product SOR3XPS6 contains solar XUV irradiances in the 0.1 to 27 nm range, as well...

  19. Charge compensation and binding energy referencing in XPS analysis

    International Nuclear Information System (INIS)

    Metson, J.B.

    1999-01-01

    Full text: The past decade has seen a number of significant advances in the capabilities of commercial X-ray Photoelectron spectrometers. Of note have been the near universal adoption of monochromatised X-ray sources, very useful advances in spatial resolution, particularly in spectroscopy, and radical developments in sample handling and automation. However one of the most significant advances has been the development of several relatively new concepts in charge compensation. Throughout the evolution of XPS, the ability to compensate for surface charging and accurately determine binding energies, particularly with electrically inhomogenous samples, has remained one of the most intractable problems. Beginning perhaps with the Kratos, 'in the lens' electrostatic mirror/electron source coupled with a magnetic snorkel lens, a number of concepts have been advanced which take a quite different conceptual approach to charge compensation. They differ in a number of quite fundamental ways to the electron flood type compensators widely used and absolutely essential with instruments based on monochromatised sources. The concept of the local return of secondary electrons to their point of emission, largely negates the problems associated with differential charging across different regions of the surface, and suggests the possibility of overcoming one of the central limitations of XPS, that is the inability to compare absolute binding energies of species in different electrical as well as chemical environments. The general status of charge compensation and the use of internal binding energy references in XPS will be reviewed, along with some practical examples of where these techniques work, and where there is clearly still room for further development. Copyright (1999) Australian X-ray Analytical Association Inc

  20. Formation of carboxy- and amide-terminated alkyl monolayers on silicon(111) investigated by ATR-FTIR, XPS, and X-ray scattering: Construction of photoswitchable surfaces

    DEFF Research Database (Denmark)

    Rück-Braun, Karola; Petersen, Michael Åxman; Michalik, Fabian

    2013-01-01

    -FTIR and XPS studies of the fulgimide samples revealed closely covered amide-terminated SAMs. Reversible photoswitching of the headgroup was read out by applying XPS, ATR-FTIR, and difference absorption spectra in the mid-IR. In XPS, we observed a reversible breathing of the amide/imide C1s and N1s signals......We have prepared high-quality, densely packed, self-assembled monolayers (SAMs) of carboxy-terminated alkyl chains on Si(111). The samples were made by thermal grafting of methyl undec-10-enoate under an inert atmosphere and subsequent cleavage of the ester functionality to disclose the carboxylic...... zigzag-like substitution pattern for the ester- and carboxy-terminated monolayer. Hydrolysis of the remaining H-Si(111) bonds at the surface furnished HO-Si(111) groups according to XPS and attenuated total reflection Fourier-transform infrared spectroscopy (ATR-FTIR) studies. The amide-terminated alkyl...

  1. XANES and XPS studies of the reduction of ammonium paramolybdate

    International Nuclear Information System (INIS)

    Halada, G.P.; Clayton, C.R.

    1991-01-01

    in situ glancing-angle x-ray reflectivity experiments were performed on electrochemical reduction products formed in a dilute paramolybdate solution on a platinum electrode. These data were compared with x-ray photoelectron spectra which showed formation of simple molybdate, pentavalent and tetravalent species at increasingly negative potentials. X-ray absorption data demonstrated changes in edge position, pre-edge structure and edge height corresponding to reduction and subsequent growth of the reduction product film at a number of the potentials examined with XPS

  2. XPS study on the surface reaction of uranium metal with carbon monoxide at 200 degree C

    International Nuclear Information System (INIS)

    Wang Xiaoling; Fu Yibei; Xie Renshou; Huang Ruiliang

    1996-12-01

    The surface reaction of uranium metal with carbon monoxide at 200 degree C has been studied by X-ray photoelectron spectroscopy (XPS). The carbon monoxide adsorption on the surface oxide layer resulted in U4f peak shifting to the lower binding energy and the content of oxygen in the oxide is decreased. O/U radio decreases with increasing the exposure of carbon monoxide to the surface layer. The investigation indicated the surface layer of uranium metal was further reduced in the atmosphere of carbon monoxide at high temperature. (3 refs., 5 figs.)

  3. XPS Studies of LSCF Interfaces after Cell Testing

    Directory of Open Access Journals (Sweden)

    Gianfranco DiGiuseppe

    2018-01-01

    Full Text Available The motivation of this investigation is to explore the possibility of using the depth profile capability of XPS to study interfaces after SOFC button cell testing. The literature uses XPS to study various cathode materials but has devoted little to the understanding of various cathode interfaces especially after testing. In this work, an SOFC button cell is first tested, and then, the LSCF cathode, barrier layer, and electrolyte are sputtered away to study the behavior of different interfaces. This work has shown that some elements have moved into other layers of the SOFC cell. It is argued that the migration of the elements is partly due to a redeposition mechanism after atoms are sputtered away, while the rest is due to interdiffusion between the SDC and YSZ layers. However, additional work is needed to better understand the mechanism by which atoms move around at different interfaces. The cell electrochemical performance is also discussed in some details but is not the focus.

  4. Speciation of uranium after microbial action by XANES and XPS

    International Nuclear Information System (INIS)

    Dodge, C.J.; Francis, A.J.; Lu, F.; Halada, G.P.; Kagwade, S.V.; Clayton, C.R.

    1993-01-01

    The speciation of radionuclides and toxic metals in wastes subjected to microbial action is important in determining the extent of stabilization in a disposal environment. As part of an ongoing study, we investigated the reduction of uranium by a Clostridium sp. using X-ray absorption neat edge spectroscopy (XANES) at the National Synchrotron Light Source (NSLS) and X-ray photoelectron spectroscopy (XPS). XPS analysis of uranyl acetate containing hexavalent uranium exhibited a binding energy of 382.0eV at the U 4f 7/2 peak. The sample incubated in the presence of bacteria was shifted to lower binding energy (380.6eV), confirming the reduction of U 6+ to U 4+ at the bacterial surface. XANES analysis, using an electron yield detector, was performed at the M v absorption edge (3d-->5f). The absorption peak energy of the sample exhibited a shift from 3551.1eV to 3550.1eV which is higher than uranium metal (3549.6eV ) but lower than U 4+ (3550.4eV). This indicates the presence of U 3+ which is probably located beneath the surface within the biomass. Anaerobic bacterial treatment of wastes containing uranyl ion can result in the stabilization of uranium

  5. XPS investigation of copper corrosion in hydro-carbonate electrolytes

    Energy Technology Data Exchange (ETDEWEB)

    Sieber, I.; Hildebrand, H.; Schmuki, P. [University Erlangen-Nuremberg, Martensstr.7, D-91058 Erlangen (Germany); Kaluzhina, S.A. [Voronezh State University, University Sq.1, 394006 Voronezh (Russian Federation)

    2004-07-01

    Problems of corrosion and effective methods of metal protection are still actual in the present days. Special interest is in copper material, which as basic component of heat exchanger constructions can corrode in contact with carbonate water. The intensity of the corrosion destruction depends on the carbon water concentration and thermal conditions in the system. The present paper provides new insights into the role of the HCO{sub 3}{sup -} - ions in the corrosion process of copper. Copper samples after anodic oxidation in 0.02 and 0.1 M NaHCO{sub 3} have been studied using XPS and SEM. The presence of carbonate compounds in the passive film in 0.1 M NaHCO{sub 3} was established by XPS analysis all over the surface. These compounds are responsible for the protective character of the passive film towards local destruction. In the 0.02 M NaHCO{sub 3} electrolyte carbonate compounds were not found at places of pit formation after multi-cycling of the sample. (authors)

  6. Combined DFT and XPS investigation of iodine anions adsorption on the sulfur terminated (001) chalcopyrite surface

    Energy Technology Data Exchange (ETDEWEB)

    Li, Kui, E-mail: likui9606@stu.xjtu.edu.cn [School of Nuclear Science and Technology, Xi’an Jiaotong University, Xi’an 710049 (China); Zhao, Yaolin, E-mail: zhaoyaolin@mail.xjtu.edu.cn [School of Nuclear Science and Technology, Xi’an Jiaotong University, Xi’an 710049 (China); Zhang, Peng, E-mail: zp32@qq.com [Sino Shaanxi Nuclear Industry Group, Xi’an 710100 (China); He, Chaohui, E-mail: hechaohui@mail.xjtu.edu.cn [School of Nuclear Science and Technology, Xi’an Jiaotong University, Xi’an 710049 (China); Deng, Jia, E-mail: djkokocase@stu.xjtu.edu.cn [School of Nuclear Science and Technology, Xi’an Jiaotong University, Xi’an 710049 (China); Ding, Shujiang, E-mail: dingsj@mail.xjtu.edu.cn [Department of Applied Chemistry, School of Science, Xi’an Jiaotong University, Xi’an 710049 (China); Shi, Weiqun, E-mail: shiwq@ihep.ac.cn [Key Laboratory of Nuclear Radiation and Nuclear Energy Technology and Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)

    2016-12-30

    Highlights: • Metal surface sites of (001)-S surface of chalcopyrite show significant chemical affinity to iodide and iodate. • The energetically favorable active site is copper for iodide adsorption and iron for iodate adsorption, respectively. • Iodate undergoes a dissociative adsorption on the copper site of chalcopyrite surface. - Abstract: The adsorption of iodine anions (iodide and iodate) on the sulfur terminated (001) chalcopyrite surface has been systematically investigated combining first-principles calculations based on density functional theory (DFT) with X-ray photoelectron spectroscopy (XPS) measurements. Based on the total energy calculations and geometric optimization, the thermodynamically preferred site was copper atom for iodide adsorption and iron atom for iodate adsorption, respectively. In the case of Cu site mode, the iodate underwent a dissociative adsorption, where one I−O bond of iodate ion was broken and the dissociative oxygen atom adsorbed on the adjacent sulphur site. Projected density of states (PDOS) analysis further clarified the interaction mechanism between active sites of chalcopyrite surface and adsorbates. In addition, full-range XPS spectra qualitatively revealed the presence of iodine on chalcopyrite surface. High resolution XPS spectra of the I 3d peaks after adsorption verified the chemical environment of iodine. The binding energies of 618.8 eV and 623.5 eV for I 3d{sub 5/2} peaks unveiled that the adsorption of iodide and iodate ions on copper-iron sulfide minerals was the result of formation of low solubility metal iodides precipitate. Also two I 3d peaks with low intensity around 618 eV and 630 eV might be related to the inorganic reduction of iodate to iodide by reducing S{sup 2−} ion of chalcopyrite.

  7. EXAFS and XPS Study of Rutile-Type Difluorides of First-Row Transition Metals

    International Nuclear Information System (INIS)

    Murai, Kei-ichiro; Suzuki, Yohei; Moriga, Toshihiro; Yoshiasa, Akira

    2007-01-01

    Although most rutile-type difluorides (MnF2, CoF2 and NiF2) have a positive thermal expansion coefficient, FeF2 has a negative thermal expansion (NTE) along the c-axis in the high temperature region. In this study, we give an explanation of that behavior with Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Photoelectron Spectroscopy (XPS) techniques. From EXAFS results, it has become apparent that the length of the share-edge (Fe-Fe) of FeF6 octahedra increased with the rise of temperature in the high temperature region. We have revealed that the force constant between nearest neighbor atoms (Fe-F) was much larger than that between second-nearest neighbor atoms (Fe-Fe) in FeF2. In XPS measurements, it was discovered that the peak of F 1s of FeF2 was located at the lowest binding energy position as compared to that of other difluorides. This means that the charge density around the F atom in FeF2 was higher than that in other difluorides. It follows from this that the share-edge repulsive force in FeF2 is larger than that in other difluorides. On account of the large repulsive force and the large force constant between nearest neighbor atoms, Fe atoms are attracted to share-edge with the rise of temperature

  8. Characterization of carbonated serpentine using XPS and TEM

    International Nuclear Information System (INIS)

    Schulze, Roland K.; Hill, Mary Ann; Field, Robert D.; Papin, Pallas A.; Hanrahan, Robert J.; Byler, Darrin D.

    2004-01-01

    With the increasing concentration volume of carbon dioxide in the atmosphere, there has been an increasing interest in carbon dioxide sequestration. One method is to store the carbon dioxide in mineral form, reacting solution dissolved CO 2 to precipitate carbonates. In order to understand whether or not such an endeavor is feasible, the carbonation reaction must first be understood. In this study, the surface of ground serpentine, untreated, heat treated and following a carbonation experiment, has been characterized using X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The results indicate that the mechanism for the reaction involves dissolution of the serpentine through the formation of an amorphous phase and subsequent precipitation of magnesite. The rate limiting step appears to be the diffusion of Mg out of the amorphous phase

  9. Surface Propensity of Atmospherically Relevant Amino Acids Studied by XPS.

    Science.gov (United States)

    Mocellin, Alexandra; Gomes, Anderson Herbert de Abreu; Araújo, Oscar Cardoso; de Brito, Arnaldo Naves; Björneholm, Olle

    2017-04-27

    Amino acids constitute an important fraction of the water-soluble organic nitrogen (WSON) compounds in aerosols and are involved in many processes in the atmosphere. In this work, we applied X-ray photoelectron spectroscopy (XPS) to study aqueous solutions of four amino acids, glycine, alanine, valine, and methionine, in their zwitterionic forms. We found that amino acids with hydrophilic side chains and smaller size, GLY and ALA, tend to stay in the bulk of the liquid, while the hydrophobic and bigger amino acids, VAL and MET, are found to concentrate more on the surface. We found experimental evidence that the amino acids have preferential orientation relative to the surface, with the hydrophobic side chain being closer to the surface than the hydrophilic carboxylate group. The observed amino acid surface propensity has implications in atmospheric science as the surface interactions play a central role in cloud droplet formation, and they should be considered in climate models.

  10. Silicon (100)/SiO2 by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, David S.; Kanyal, Supriya S.; Madaan, Nitesh; Vail, Michael A.; Dadson, Andrew; Engelhard, Mark H.; Linford, Matthew R.

    2013-09-25

    Silicon (100) wafers are ubiquitous in microfabrication and, accordingly, their surface characteristics are important. Herein, we report the analysis of Si (100) via X-ray photoelectron spectroscopy (XPS) using monochromatic Al K radiation. Survey scans show that the material is primarily silicon and oxygen, and the Si 2p region shows two peaks that correspond to elemental silicon and silicon dioxide. Using these peaks the thickness of the native oxide (SiO2) was estimated using the equation of Strohmeier.1 The oxygen peak is symmetric. The material shows small amounts of carbon, fluorine, and nitrogen contamination. These silicon wafers are used as the base material for subsequent growth of templated carbon nanotubes.

  11. XPS analysis of aluminosilicate microspheres bioactivity tested in vitro

    Energy Technology Data Exchange (ETDEWEB)

    Todea, M.; Vanea, E. [Faculty of Physics and Institute of Interdisciplinary Research on Bio-Nano-Sciences, Babes Bolyai University, Cluj-Napoca 400084 (Romania); Bran, S. [University of Medicine and Pharmacy “Iuliu Haţieganu”, Department of Cranio-Maxillofacial Surgery, 400029 Cluj-Napoca (Romania); Berce, P. [Technical University of Cluj-Napoca, Faculty of Machine Building and National Centre of Rapid Prototyping, 400641 Cluj-Napoca (Romania); Simon, S., E-mail: simons@phys.ubbcluj.ro [Faculty of Physics and Institute of Interdisciplinary Research on Bio-Nano-Sciences, Babes Bolyai University, Cluj-Napoca 400084 (Romania)

    2013-04-01

    The study aims to characterize surface properties of aluminosilicate microspheres incorporating yttrium, with potential biomedical applications. Micrometric particles of spherical shape were obtained by spray drying method. The behavior of aluminosilicate microspheres without yttrium and with yttrium was investigated under in vitro conditions, by seven days incubation in simulated body fluid (SBF). The surface elemental composition and the atomic environments on outermost layer of the microspheres, prior to and after incubation in SBF were evaluated by X-ray photoelectron spectroscopy (XPS) in order to investigate their bioactivity. The results were analyzed to underline the effect of yttrium addition on surface properties of the aluminosilicate microspheres and implicitly on the behavior of the samples in simulated body environments.

  12. An XPS round robin investigation on analysis of wood pulp fibres and filter paper

    Science.gov (United States)

    Johansson, Leena-Sisko; Campbell, J. M.; Fardim, Pedro; Hultén, Anette Heijnesson; Boisvert, Jean-Philippe; Ernstsson, Marie

    2005-06-01

    X-ray photoelectron spectroscopy (XPS) has been applied to pulp and paper research for decades. However, there has been no attempt to standardise or even systematically compare experimental and analysis procedures, even though it is known that fibrous, nature-derived and insulating fibre materials pose remarkable challenges to reliable surface analysis. The experimental problems are mainly linked with neutralisation, energy resolution, contamination and X-ray induced degradation. We have tested applicability, reliability and reproducibility of XPS analysis on real pulp samples with varying lignin and extractives contents in a small round robin investigation. We also tested the instrumental set-ups with an acetone-extracted filter paper, used as a reference sample. The data, collected at four different laboratories with state-of-the-art instruments indicate that reproducible results can be obtained, despite minor differences in experimental and analysis procedures. However, we found that a specified sample handling procedure and limited X-ray exposure are crucial for reproducible, reliable data. Based on the round robin data we recommend dose restricted monochromatic measurements, a cellulosic in situ reference and a consistent sample handling procedure. The data confirms that a paper-based reference material and the correlation of high-resolution C 1s data with O/C atomic ratios can be used in testing instruments and experimental set-ups for pulp and paper materials.

  13. Label-free cellular structure imaging with 82 nm lateral resolution using an electron-beam excitation-assisted optical microscope.

    Science.gov (United States)

    Fukuta, Masahiro; Masuda, Yuriko; Inami, Wataru; Kawata, Yoshimasa

    2016-07-25

    We present label-free and high spatial-resolution imaging for specific cellular structures using an electron-beam excitation-assisted optical microscope (EXA microscope). Images of the actin filament and mitochondria of stained HeLa cells, obtained by fluorescence and EXA microscopy, were compared to identify cellular structures. Based on these results, we demonstrated the feasibility of identifying label-free cellular structures at a spatial resolution of 82 nm. Using numerical analysis, we calculated the imaging depth region and determined the spot size of a cathodoluminescent (CL) light source to be 83 nm at the membrane surface.

  14. Plasma-oxidation of Ge(100)-surfaces characterized by MIES, UPS and XPS

    Energy Technology Data Exchange (ETDEWEB)

    Wegewitz, Lienhard; Dahle, Sebastian; Maus-Friedrichs, Wolfgang [Institut fuer Energieforschung und Physikalische Technologien, Technische Universitaet Clausthal, Leibnizstr. 4, 38678 Clausthal-Zellerfeld (Germany); Hoefft, Oliver; Endres, Frank [Institut fuer Mechanische Verfahrenstechnik, Technische Universitaet Clausthal, Arnold-Sommerfeld-Str. 6, 38678 Clausthal-Zellerfeld (Germany); Vioel, Wolfgang [HAWK Goettingen, Fakultaet Naturwissenschaften und Technik, Von-Ossietzky-Str. 99, 37085 Goettingen (Germany)

    2011-07-01

    Cleaning and passivation of Germanium surfaces is of tremendous technological interest. Germanium has various applications, for example in complementary metal-oxide-semiconductor elements. It turned out to be difficult to prepare contamination free Germanium surfaces by methods of wet chemistry. Several attempts have been made preparing such surfaces by different plasma treatments. We report cleaning and passivation of Ge(100)-surfaces by dielectric barrier discharge plasma at ambient temperature in oxygen and in air studied by Metastable Induced Electron Spectroscopy (MIES) and Photoelectron Spectroscopy (UPS(He I) and XPS). The plasma treatment is carried out in a special high-vacuum chamber which operates up to ambient pressure and is directly connected to the ultra-high vacuum chamber including the analysis equipment. In summary the air plasma treatment as well as the oxygen plasma treatment result in contamination free GeO{sub 2} covered surfaces.

  15. Stability of boron-doped graphene/copper interface: DFT, XPS and OSEE studies

    Science.gov (United States)

    Boukhvalov, D. W.; Zhidkov, I. S.; Kukharenko, A. I.; Slesarev, A. I.; Zatsepin, A. F.; Cholakh, S. O.; Kurmaev, E. Z.

    2018-05-01

    Two different types of boron-doped graphene/copper interfaces synthesized using two different flow rates of Ar through the bubbler containing the boron source were studied. X-ray photoelectron spectra (XPS) and optically stimulated electron emission (OSEE) measurements have demonstrated that boron-doped graphene coating provides a high corrosion resistivity of Cu-substrate with the light traces of the oxidation of carbon cover. The density functional theory calculations suggest that for the case of substitutional (graphitic) boron-defect only the oxidation near boron impurity is energetically favorable and creation of the vacancies that can induce the oxidation of copper substrate is energetically unfavorable. In the case of non-graphitic boron defects oxidation of the area, a nearby impurity is metastable that not only prevent oxidation but makes boron-doped graphene. Modeling of oxygen reduction reaction demonstrates high catalytic performance of these materials.

  16. Studies of irradiated zircaloy fuel sheathing using XPS

    International Nuclear Information System (INIS)

    Chan, P.K.; Irving, K.G.; Hocking, W.H.; Duclos, A.M.; Gerwing, A.F.

    1995-01-01

    The preliminary results reported here support the hypothesis that CANLUB graphite coating reduces the rate at which oxygen can react with fuel sheathing. X-ray photoelectron spectroscopic (XPS) characterization of Zircaloy sheathing obtained from extended-burnup Bruce-type elements (BDL-406-XY (555 MW.h/kgU) and BDL-406-AAH (731 MW.h/kgU)) irradiated in NRU indicates that CANLUB may reduce fuel sheath oxidation, and hence that fission-liberated oxygen may remain in the fuel. Chemical shifts in the Zr 3d spectra suggest that a stoichiometric (ZrO 2 ) oxide film was formed only on Zircaloy in direct contact with fuel. Particulate fuel adhering to the sheath was also determined to be systematically more oxidized on surfaces with CANLUB than on those without it. The unique association of tin on sheathing specimens with the non-CANLUB-coated specimens might also suggest that the tin had segregated from the sheathing. It must be emphasized that further experiments are required to better define the effect of CANLUB on fuel oxidation. (author). 14 refs., 1 tab., 3 figs

  17. The assessment of metal surface cleanliness by XPS

    CERN Document Server

    Scheuerlein, C

    2006-01-01

    The most commonly used quantity to characterize surface cleanliness through X-ray photoemission spectroscopy (XPS) measurements is the so-called relative atomic surface concentration of carbon (at.% C). We have investigated the relationship between at.% C values and the C 1s peak area on Cu and we find a nearly linear behaviour in the range 15–80 at.% C. Correction factors for the measured at.% C values that enable a comparison of the cleanliness level of different materials, notably Cu, Al and stainless steel, have been determined experimentally. The influence of the storage time and method on the degree of re-contamination of initially clean Cu has been examined. The carbon contamination on clean metallic Cu increases abruptly to some 20 at.% C upon air exposure and continues to increase with storage time in air. Storage in polymer bags can lead to up to 70 at.% C after 1 month, whereas storage in aluminium foil can preserve an acceptable surface cleanliness for a similar storage time.

  18. Studies of irradiated zircaloy fuel sheathing using XPS

    Energy Technology Data Exchange (ETDEWEB)

    Chan, P K; Irving, K G [Atomic Energy of Canada Ltd., Chalk River, ON (Canada); Hocking, W H; Duclos, A M; Gerwing, A F [Atomic Energy of Canada Ltd., Pinawa, MB (Canada). Whiteshell Labs.

    1996-12-31

    The preliminary results reported here support the hypothesis that CANLUB graphite coating reduces the rate at which oxygen can react with fuel sheathing. X-ray photoelectron spectroscopic (XPS) characterization of Zircaloy sheathing obtained from extended-burnup Bruce-type elements (BDL-406-XY (555 MW.h/kgU) and BDL-406-AAH (731 MW.h/kgU)) irradiated in NRU indicates that CANLUB may reduce fuel sheath oxidation, and hence that fission-liberated oxygen may remain in the fuel. Chemical shifts in the Zr 3d spectra suggest that a stoichiometric (ZrO{sub 2}) oxide film was formed only on Zircaloy in direct contact with fuel. Particulate fuel adhering to the sheath was also determined to be systematically more oxidized on surfaces with CANLUB than on those without it. The unique association of tin on sheathing specimens with the non-CANLUB-coated specimens might also suggest that the tin had segregated from the sheathing. It must be emphasized that further experiments are required to better define the effect of CANLUB on fuel oxidation. (author). 14 refs., 1 tab., 3 figs.

  19. Sub-nanometer resolution XPS depth profiling: Sensing of atoms

    Energy Technology Data Exchange (ETDEWEB)

    Szklarczyk, Marek, E-mail: szklarcz@chem.uw.edu.pl [Faculty of Chemistry, University of Warsaw, ul. Pasteura 1, 02-093 Warsaw (Poland); Shim-Pol, ul. Lubomirskiego 5, 05-080 Izabelin (Poland); Macak, Karol; Roberts, Adam J. [Kratos Analytical Ltd, Wharfside, Trafford Wharf Road, Manchester, M17 1GP (United Kingdom); Takahashi, Kazuhiro [Kratos XPS Section, Shimadzu Corp., 380-1 Horiyamashita, Hadano, Kanagawa 259-1304 (Japan); Hutton, Simon [Kratos Analytical Ltd, Wharfside, Trafford Wharf Road, Manchester, M17 1GP (United Kingdom); Głaszczka, Rafał [Shim-Pol, ul. Lubomirskiego 5, 05-080 Izabelin (Poland); Blomfield, Christopher [Kratos Analytical Ltd, Wharfside, Trafford Wharf Road, Manchester, M17 1GP (United Kingdom)

    2017-07-31

    Highlights: • Angle resolved photoelectron depth profiling of nano thin films. • Sensing atomic position in SAM films. • Detection of direction position of adsorbed molecules. - Abstract: The development of a method capable of distinguishing a single atom in a single molecule is important in many fields. The results reported herein demonstrate sub-nanometer resolution for angularly resolved X-ray photoelectron spectroscopy (ARXPS). This is made possible by the incorporation of a Maximum Entropy Method (MEM) model, which utilize density corrected electronic emission factors to the X-ray photoelectron spectroscopy (XPS) experimental results. In this paper we report on the comparison between experimental ARXPS results and reconstructed for both inorganic and organic thin film samples. Unexpected deviations between experimental data and calculated points are explained by the inaccuracy of the constants and standards used for the calculation, e.g. emission factors, scattering intensity and atomic density through the studied thickness. The positions of iron, nitrogen and fluorine atoms were determined in the molecules of the studied self-assembled monolayers. It has been shown that reconstruction of real spectroscopic data with 0.2 nm resolution is possible.

  20. The equivalent width as a figure of merit for XPS narrow scans

    International Nuclear Information System (INIS)

    Singh, Bhupinder; Velázquez, Daniel; Terry, Jeff; Linford, Matthew R.

    2014-01-01

    Highlights: • We introduce a new figure of merit for XPS narrow scans: the equivalent width (EW XPS ). • EW XPS is less subjective and involves lesser user bias than traditional peak fitting. • EW XPS is responsive to changes in chemical states of materials. • EW XPS could be used for quality control and comparing spectra from similar samples. • EW XPS has the potential to be part of an expert software system for machine interpretation of spectra. - Abstract: X-ray Photoelectron Spectroscopy (XPS) is a widely used surface analytical tool that provides information about the near surface regions of materials. And while indispensable for XPS data analysis, peak fitting of narrow scans is often a fairly subjective exercise. Herein we introduce the equivalent width (EW) as an additional and less subjective figure of merit for XPS narrow scans. We believe that this parameter will prove particularly useful for analyzing series of similar or nominally identical spectra, perhaps as a component of an expert software system for the machine interpretation of spectra. It also appears to be useful, shedding light on the chemical state of materials, when additional information about a sample is known. The EW XPS is simply defined as the area of a narrow scan divided by the height of the maximum of its peak envelope. To limit any ambiguity in EW XPS for a series of spectra, we may also list the peak position of the maximum of the envelope (PE max ). The potential usefulness and limitations of the EW XPS and PE max parameters are demonstrated by their application to the narrow scans of: (i) four sets of ozone-treated carbon nanotubes (EW XPS ∼ 2.11–2.16 eV for a Shirley background, and up to 2.88 eV for no background, PE max ∼ 284.4–284.5 eV), (ii) a series of silicon wafers with different oxide thicknesses (EW XPS ∼ 1.5–2.8 eV, PE max ∼ 99–103 eV), (iii) hydrogen-terminated silicon before and after derivatization with pentyl groups, and after annealing of

  1. The equivalent width as a figure of merit for XPS narrow scans

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Bhupinder [Department of Chemistry and Biochemistry, C-100 BNSN, Brigham Young University, Provo, UT 84602 (United States); Velázquez, Daniel [Department of Physics, Illinois Institute of Technology, Chicago, IL 60616 (United States); Terry, Jeff, E-mail: terryj@iit.edu [Department of Physics, Illinois Institute of Technology, Chicago, IL 60616 (United States); Linford, Matthew R., E-mail: mrlinford@chem.byu.edu [Department of Chemistry and Biochemistry, C-100 BNSN, Brigham Young University, Provo, UT 84602 (United States)

    2014-12-15

    Highlights: • We introduce a new figure of merit for XPS narrow scans: the equivalent width (EW{sub XPS}). • EW{sub XPS} is less subjective and involves lesser user bias than traditional peak fitting. • EW{sub XPS} is responsive to changes in chemical states of materials. • EW{sub XPS} could be used for quality control and comparing spectra from similar samples. • EW{sub XPS} has the potential to be part of an expert software system for machine interpretation of spectra. - Abstract: X-ray Photoelectron Spectroscopy (XPS) is a widely used surface analytical tool that provides information about the near surface regions of materials. And while indispensable for XPS data analysis, peak fitting of narrow scans is often a fairly subjective exercise. Herein we introduce the equivalent width (EW) as an additional and less subjective figure of merit for XPS narrow scans. We believe that this parameter will prove particularly useful for analyzing series of similar or nominally identical spectra, perhaps as a component of an expert software system for the machine interpretation of spectra. It also appears to be useful, shedding light on the chemical state of materials, when additional information about a sample is known. The EW{sub XPS} is simply defined as the area of a narrow scan divided by the height of the maximum of its peak envelope. To limit any ambiguity in EW{sub XPS} for a series of spectra, we may also list the peak position of the maximum of the envelope (PE{sub max}). The potential usefulness and limitations of the EW{sub XPS} and PE{sub max} parameters are demonstrated by their application to the narrow scans of: (i) four sets of ozone-treated carbon nanotubes (EW{sub XPS} ∼ 2.11–2.16 eV for a Shirley background, and up to 2.88 eV for no background, PE{sub max} ∼ 284.4–284.5 eV), (ii) a series of silicon wafers with different oxide thicknesses (EW{sub XPS} ∼ 1.5–2.8 eV, PE{sub max} ∼ 99–103 eV), (iii) hydrogen-terminated silicon before

  2. Laser interference lithography with highly accurate interferometric alignment

    NARCIS (Netherlands)

    van Soest, Frank J.; van Wolferen, Hendricus A.G.M.; Hoekstra, Hugo; de Ridder, R.M.; Worhoff, Kerstin; Lambeck, Paul

    It is shown experimentally that in laser interference lithography, by using a reference grating, respective grating layers can be positioned with high relative accuracy. A 0.001 degree angular and a few nanometers lateral resolution have been demonstrated.

  3. Thermally Evaporated Iron (Oxide) on an Alumina Barrier Layer, by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Madaan, Nitesh; Kanyal, Supriya S.; Jensen, David S.; Vail, Michael A.; Dadson, Andrew; Engelhard, Mark H.; Linford, Matthew R.

    2013-09-06

    We report the XPS characterization of a thermally evaporated iron thin film (6 nm) deposited on an Si/SiO_2/Al_2O_3 substrate using Al Ka X-rays. An XPS survey spectrum, narrow Fe 2p scan, narrow O 1s, and valence band scan are shown.

  4. XPS studies of SiO2 surface layers formed by oxygen ion implantation into silicon

    International Nuclear Information System (INIS)

    Schulze, D.; Finster, J.

    1983-01-01

    SiO 2 surface layers of 160 nm thickness formed by 16 O + ion implantation into silicon are examined by X-ray photoelectron spectroscopy measurements into the depth after a step-by-step chemical etching. The chemical nature and the thickness of the transition layer were determined. The results of the XPS measurements show that the outer surface and the bulk of the layers formed by oxygen implantation and subsequent high temperature annealing consist of SiO 2 . There is no evidence for Si or SiO/sub x/ (0 2 and Si is similar to that of thin grown oxide layers. Only its thickness is somewhat larger than in thermal oxide

  5. XPS Protocol for the Characterization of Pristine and Functionalized Single Wall Carbon Nanotubes

    Science.gov (United States)

    Sosa, E. D.; Allada, R.; Huffman, C. B.; Arepalli, S.

    2009-01-01

    Recent interest in developing new applications for carbon nanotubes (CNT) has fueled the need to use accurate macroscopic and nanoscopic techniques to characterize and understand their chemistry. X-ray photoelectron spectroscopy (XPS) has proved to be a useful analytical tool for nanoscale surface characterization of materials including carbon nanotubes. Recent nanotechnology research at NASA Johnson Space Center (NASA-JSC) helped to establish a characterization protocol for quality assessment for single wall carbon nanotubes (SWCNTs). Here, a review of some of the major factors of the XPS technique that can influence the quality of analytical data, suggestions for methods to maximize the quality of data obtained by XPS, and the development of a protocol for XPS characterization as a complementary technique for analyzing the purity and surface characteristics of SWCNTs is presented. The XPS protocol is then applied to a number of experiments including impurity analysis and the study of chemical modifications for SWCNTs.

  6. Use of XPS to clarify the Hall coefficient sign variation in thin niobium layers buried in silicon

    Energy Technology Data Exchange (ETDEWEB)

    Demchenko, Iraida N., E-mail: demch@ifpan.edu.pl [Institute of Physics, Polish Academy of Sciences, Aleja Lotnikow 32/46, PL-02668 Warsaw (Poland); Lisowski, Wojciech [Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw (Poland); Syryanyy, Yevgen [Institute of Physics, Polish Academy of Sciences, Aleja Lotnikow 32/46, PL-02668 Warsaw (Poland); Melikhov, Yevgen [Institute of Physics, Polish Academy of Sciences, Aleja Lotnikow 32/46, PL-02668 Warsaw (Poland); School of Engineering, Cardiff University, Newport Rd., Cardiff, CF24 3AA (United Kingdom); Zaytseva, Iryna; Konstantynov, Pavlo [Institute of Physics, Polish Academy of Sciences, Aleja Lotnikow 32/46, PL-02668 Warsaw (Poland); Chernyshova, Maryna [Institute of Plasma Physics and Laser Microfusion, Hery Street 23, 01-497 Warsaw (Poland); Cieplak, Marta Z. [Institute of Physics, Polish Academy of Sciences, Aleja Lotnikow 32/46, PL-02668 Warsaw (Poland)

    2017-03-31

    Highlights: • HR XPS spectra of Nb 3d, Si 2p, O 1s were probed for Si/Nb/Si trilayers prepared by magnetron sputtering to clarify the Hall coefficient variation as a function of Nb layer thickness. • Strong boundary scattering, enhanced by the presence of silicon ions in the layer close to the interface/s is a main factor leading to sign change of the Hall coefficient. • Theoretical concentration/depth profile as a function of sputtering determined by SESSA after optimization of the model system gives good agreement with experiment. - Abstract: Si/Nb/Si trilayers formed with 9.5 and 1.3 nm thick niobium layer buried in amorphous silicon were prepared by magnetron sputtering and studied using XPS depth-profile techniques in order to investigate the change of Hall coefficient sign with thickness. The analysis of high-resolution (HR) XPS spectra revealed that the thicker layer sample has sharp top interface and metallic phase of niobium, thus holes dominate the transport. In contrast, the analysis indicates that the thinner layer sample has a Nb-rich mixed alloy formation at the top interface. The authors suggest that the main effect leading to a change of sign of the Hall coefficient for the thinner layer sample (which is negative contrary to the positive sign for the thicker layer sample) may be related to strong boundary scattering enhanced by the presence of silicon ions in the layer close to the interface/s. The depth-profile reconstruction was performed by SESSA software tool confirming that it can be reliably used for quantitative analysis/interpretation of experimental XPS data.

  7. Study on the surface chemical properties of UV excimer laser irradiated polyamide by XPS, ToF-SIMS and CFM

    International Nuclear Information System (INIS)

    Yip, Joanne; Chan, Kwong; Sin, Kwan Moon; Lau, Kai Shui

    2002-01-01

    Polyamide (nylon 6) was irradiated by a pulsed ultraviolet (UV) excimer laser with a fluence below its ablation threshold. Chemical modifications on laser treated nylon were studied by X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (Tof-SIMS) and chemical force microscopy (CFM). XPS study provides information about changes in chemical composition and the chemical-state of atom types on the fiber surface. The high sensitivity of ToF-SIMS to the topmost layers was used to detect crosslinking after the laser treatment. Gold-coated AFM tips modified with -COOH terminated self-assembled alkanethiol monolayers (SAMs) were used to measure adhesion forces on the untreated and laser treated samples. XPS results revealed that the irradiated samples have higher oxygen content than prior to laser irradiation. Tof-SIMS analysis illustrated that carbonyl groups in nylon 6 decrease significantly but hydroxyl groups increase after low-fluence laser irradiation. The adhesion force measurements by CFM showed spatial distribution of hydroxyl groups on nylon 6 after the laser treatment

  8. Heat capacity measurements and XPS studies on uranium-lanthanum mixed oxides

    International Nuclear Information System (INIS)

    Venkata Krishnan, R.; Mittal, V.K.; Babu, R.; Senapati, Abhiram; Bera, Santanu; Nagarajan, K.

    2011-01-01

    Research highlights: → Heat capacity measurements were carried out on (U 1-y La y )O 2±x (y = 0.2, 0.4, 0.6, and 0.8) using differential scanning calorimeter (DSC) in the temperature range 298-800 K. → Enthalpy increment measurements were carried out on the above solid solution using high temperature drop calorimetry in the temperature range 800-1800 K. → Chemical states of U and La in the solid solutions of mixed oxides were determined using X-ray photoelectron spectroscopy (XPS). → The anomalous increase in the heat capacity is attributed to certain thermal excitation process namely Frenkel pair defect of oxygen. → From the XPS investigation, it is observed that the O/M ratio at the surface is higher than that to the bulk. → In uranium rich mixed oxide samples, the surface O/M is greater than 2 whereas that in La rich mixed oxides, it is less than 2, though the bulk O/M in all the samples are less than 2. - Abstract: Heat capacity measurements were carried out on (U 1-y La y )O 2±x (y = 0.2, 0.4, 0.6, and 0.8) using differential scanning calorimeter (DSC) in the temperature range 298-800 K. Enthalpy increment measurements were carried out on the above solid solutions using high temperature drop calorimetry in the temperature range 800-1800 K. Chemical states of U and La in the solid solutions of mixed oxides were determined using X-ray photoelectron spectroscopy (XPS). Oxygen to metal ratios of (U 1-y La y )O 2±x were estimated from the ratios of different chemical states of U present in the sample. Anomalous increase in the heat capacity is observed for (U 1-y La y )O 2±x (y = 0.4, 0.6 and 0.8) with onset temperatures in the range of 1000-1200 K. The anomalous increase in the heat capacity is attributed to certain thermal excitation process, namely, Frenkel pair defect of oxygen. The heat capacity value of (U 1-y La y )O 2±x (y = 0.2, 0.4, 0.6, and 0.8) at 298 K are 65.3, 64.1, 57.7, 51.9 J K -1 mol -1 , respectively. From the XPS investigations

  9. 13C NMR and XPS characterization of anion adsorbent with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse

    International Nuclear Information System (INIS)

    Cao, Wei; Wang, Zhenqian; Zeng, Qingling; Shen, Chunhua

    2016-01-01

    Highlights: • 13 C NMR and XPS were successfully used to characterize quaternary ammonium groups in the surface of crop straw based anion adsorbents. • The results obtained from different kinds of crop straw material clearly confirmed the presence of quaternary ammonium groups. • The composition of C-groups and N-groups also were determined by curving fitting of high-resolution XPS C1 and N1 spectra. - Abstract: Despite amino groups modified crop straw has been intensively studied as new and low-cost adsorbent for removal of anionic species from water, there is still a lack of clear characterization for amino groups, especially quaternary ammonium groups in the surface of crop straw. In this study, we used 13 C NMR and XPS technologies to characterize adsorbents with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse. 13 C NMR spectra clearly showed the presence of quaternary ammonium groups in lignocelluloses structure of modified crop straw. The increase of nitrogen observed in XPS survey spectra also indicated the existence of quaternary ammonium group in the surface of the adsorbents. The curve fitting of high-resolution XPS N1s and C1s spectra were conducted to probe the composition of nitrogen and carbon contained groups, respectively. The results showed the proportion of quaternary ammonium group significantly increased in the prepared adsorbent’s surface that was dominated by methyl/methylene, hydroxyl, quaternary ammonium, ether and carbonyl groups. This study proved that 13 C NMR and XPS could be successfully utilized for characterization of quaternary ammonium modified crop straw adsorbents.

  10. {sup 13}C NMR and XPS characterization of anion adsorbent with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Wei, E-mail: weicao@hqu.edu.cn; Wang, Zhenqian; Zeng, Qingling; Shen, Chunhua

    2016-12-15

    Highlights: • {sup 13}C NMR and XPS were successfully used to characterize quaternary ammonium groups in the surface of crop straw based anion adsorbents. • The results obtained from different kinds of crop straw material clearly confirmed the presence of quaternary ammonium groups. • The composition of C-groups and N-groups also were determined by curving fitting of high-resolution XPS C1 and N1 spectra. - Abstract: Despite amino groups modified crop straw has been intensively studied as new and low-cost adsorbent for removal of anionic species from water, there is still a lack of clear characterization for amino groups, especially quaternary ammonium groups in the surface of crop straw. In this study, we used {sup 13}C NMR and XPS technologies to characterize adsorbents with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse. {sup 13}C NMR spectra clearly showed the presence of quaternary ammonium groups in lignocelluloses structure of modified crop straw. The increase of nitrogen observed in XPS survey spectra also indicated the existence of quaternary ammonium group in the surface of the adsorbents. The curve fitting of high-resolution XPS N1s and C1s spectra were conducted to probe the composition of nitrogen and carbon contained groups, respectively. The results showed the proportion of quaternary ammonium group significantly increased in the prepared adsorbent’s surface that was dominated by methyl/methylene, hydroxyl, quaternary ammonium, ether and carbonyl groups. This study proved that {sup 13}C NMR and XPS could be successfully utilized for characterization of quaternary ammonium modified crop straw adsorbents.

  11. A comparative study of Mg and Pt contacts on semi-insulating GaAs: Electrical and XPS characterization

    Energy Technology Data Exchange (ETDEWEB)

    Dubecký, F., E-mail: elekfdub@savba.sk [Institute of Electrical Engineering, SAS, Dúbravská cesta 9, Bratislava, SK-84104 (Slovakia); Kindl, D.; Hubík, P. [Institute of Physics CAS, v.v.i., Cukrovarnická 10, CZ-16200 Prague (Czech Republic); Mičušík, M. [Polymer Institute, SAS, Dúbravská cesta 9, Bratislava, SK-84541 (Slovakia); Dubecký, M. [Department of Physics, Faculty of Science, University of Ostrava, 30. dubna 22, CZ-70103 Ostrava 1 (Czech Republic); Boháček, P.; Vanko, G. [Institute of Electrical Engineering, SAS, Dúbravská cesta 9, Bratislava, SK-84104 (Slovakia); Gombia, E. [IMEM-CNR, Parco area delle Scienze 37/A, Parma, I-43010 (Italy); Nečas, V. [Faculty of Electrical Engineering and Information Technology, SUT, Ilkovičova 3, Bratislava, SK-81219 (Slovakia); Mudroň, J. [Department of Electronics, Academy of Armed Forces, Demänová 393, Liptovský Mikuláš, SK-03106 (Slovakia)

    2017-02-15

    Highlights: • Explored were diodes with full-area low/high work function metal contacts on semi-insulating GaAs (S). • The Mg-S-Mg diode is promising for radiation detectors for its low high-field current. • The XPS analysis of Mg-S interface shows presence of MgO instead of Mg metal. - Abstract: We present a comparative study of the symmetric metal-SI GaAs-metal (M-S-M) diodes with full-area contacts on both device sides, in order to demonstrate the effect of contact metal work function in a straightforward way. We compare the conventional high work function Pt contact versus the less explored low work function Mg contact. The Pt-S-Pt, Mg-S-Mg and mixed Mg-S-Pt structures are characterized by the current-voltage measurements, and individual Pt-S and Mg-S contacts are investigated by the X-ray photoelectron spectroscopy (XPS). The transport measurements of Mg-S-Pt structure show a significant current decrease at low bias while the Mg-S-Mg structure shows saturation current at high voltages more than an order of magnitude lower with respect to the Pt-S-Pt reference. The phenomena observed in Mg-containing samples are explained by the presence of insulating MgO layer at the M-S interface, instead of the elementary Mg, as confirmed by the XPS analysis. Alternative explanations of the influence of MgO layer on the effective resistance of the structures are presented. The reported findings have potential applications in M-S-M sensors and radiation detectors based on SI GaAs.

  12. Speciation of uranium in minerals by Sem, Tem, μ-PIXE, XPS and XAFS

    International Nuclear Information System (INIS)

    Toshihiko Ohnuki; Hiroshi Isobe; Tomihiro Kamiya; Takuro Sakai; Takashi Murakami

    2001-01-01

    Many kinds of electromagnetic waves and particle beams are used as analytical probes for the investigation of uranium-mineralogy and speciation. The representatives of the probes are SEM, TEM, μ-PIRE, XPS and XAFS. Each of these analytical probes has its own advantages and disadvantages. We have performed studies to compare the advantages and disadvantages on the basis of the analysis of the distribution and speciation of U containing rock samples collected at the Koongarra uranium deposit, Australia. The spatial resolutions of the probes are in the order of TEM>SEM, μ-PIXE>XFAS, XPS. The lower detection limits of the probes are in the order of μ-PIXE< TEM, SEM< XFAS, XPS. Oxidation state of U was determined by XFAS and XPS. These results indicate that combination of the above probes can give us sufficient data on U speciation not only in natural rock samples but in solid samples obtained in the laboratory. (authors)

  13. Research and industrial application of x-ray photoelectron spectroscopy (XPS) in Malaysia

    International Nuclear Information System (INIS)

    Mohd Ambar Yarmo; Abd Razak Daud; Abdul Kariem Arof

    2000-01-01

    As a developing country, Malaysia is fully committed to research and development especially for industrial development. One of priority fields is advanced materials and surface analysis of such materials is an important aspect in research. Among the tools for surface science analysis is x-ray photoelectron spectroscopy (XPS) which can be considered new to this country. The industrial sector is also keen to solve their problems and developing their products using XPS. The microelectronic and electrical industries are interested in solving problems related to metal-metal joining , gold silica peeling, surface corrosion and surface coating. The glove industry uses XPS to solve problems due to staining and color fading of their products. Research conducted in universities and research institutes that mainly deal with catalysis, membranes for fuel cells, sensors, batteries, corrosion phenomena and interface interaction in coating finds XPS a useful technique for surface studies. Specific examples from various sectors will be presented in this paper. (Author)

  14. Instrument-related geometrical factors affecting the intensity in XPS and ARXPS experiments

    Energy Technology Data Exchange (ETDEWEB)

    Herrera-Gomez, A., E-mail: aherrera@qro.cinvestav.mx [CINVESTAV-Unidad Queretaro, Queretaro 76230 (Mexico); Aguirre-Tostado, F.S. [Centro de Investigacion en Materiales Avanzados, Apodaca, Nuevo Leon 66600 (Mexico); Mani-Gonzalez, P.G.; Vazquez-Lepe, M.; Sanchez-Martinez, A.; Ceballos-Sanchez, O. [CINVESTAV-Unidad Queretaro, Queretaro 76230 (Mexico); Wallace, R.M. [Materials Science and Engineering, University of Texas at Dallas, Richardson, TX 75080 (United States); Conti, G.; Uritsky, Y. [Applied Materials, Santa Clara, CA 95054 (United States)

    2011-11-15

    Highlights: {yields} Instrument geometrical-factors affecting the XPS angular dependence are described. {yields} The geometrical factors in XPS instruments are transferable to other systems. {yields} Practical protocols are presented for assessing the size of analysis area and volume. {yields} Practical protocols are presented for assessing the size of the X-ray beam spot. {yields} Practical protocols are described for assessing the manipulator's axis of rotation. - Abstract: The angular dependence of the X-ray photoelectron spectroscopy (XPS) signal is influenced not only by the electron take-off angle, but also by instrument-related geometrical factors. The XPS signal is, in fact, integrated over the overlap between the X-ray beam, the spectrometer analysis volume, and the sample surface. This overlap depends on the size and shape of the spectrometer analysis volume and X-ray beam, as well as on their relative orientation. In this paper it is described the models and protocols for the characterization of the parameters defining the geometry of an XPS instrument. The protocols include practical methods for assessing the spectrometer analysis area and the X-ray beam spot dimension. Simple systems consisting of flat and 'thick' gold films on silicon wafers were employed. The parameters found with those samples are transferable to other more complex systems since they are geometrical in nature. The method allows for the prediction of the actual intensity of XPS peaks, hence removing the need of normalizing the peak areas to the area of a determined substrate peak. The associated reduction of the uncertainty in half is of special importance since the quantitative analysis of angle-resolved XPS data could be very sensitive to noise. Two rotating and one non-rotating XPS instruments are described. Some examples of the applications of the method are also provided.

  15. Combined PIXE and XPS analysis on republican and imperial Roman coins

    International Nuclear Information System (INIS)

    Dacca, A.; Prati, P.; Zucchiatti, A.; Lucarelli, F.; Mando, P.A.; Gemme, G.; Parodi, R.; Pera, R.

    2000-01-01

    A combined PIXE and XPS analysis has been performed on a few Roman coins of the republican and imperial age. The purpose was to investigate via XPS the nature and extent of patina in order to be capable of extracting PIXE data relative to the coins bulk. The inclusion of elements from the surface layer, altered by oxidation and inclusion, is a known source of uncertainty in PIXE analyses of coins, performed to assess the composition and the provenance

  16. Generalized molybdenum oxide surface chemical state XPS determination via informed amorphous sample model

    Energy Technology Data Exchange (ETDEWEB)

    Baltrusaitis, Jonas, E-mail: job314@lehigh.edu [Department of Chemical Engineering, Lehigh University, B336 Iacocca Hall, 111 Research Drive, Bethlehem, PA 18015 (United States); PhotoCatalytic Synthesis group, MESA+ Institute for Nanotechnology, Faculty of Science and Technology, University of Twente, Meander 229, P.O. Box 217, 7500 AE Enschede (Netherlands); Mendoza-Sanchez, Beatriz [CRANN, Chemistry School, Trinity College Dublin, Dublin (Ireland); Fernandez, Vincent [Institut des Matériaux Jean Rouxel, 2 rue de la Houssinière, BP 32229, F-44322 Nantes Cedex 3 (France); Veenstra, Rick [PhotoCatalytic Synthesis group, MESA+ Institute for Nanotechnology, Faculty of Science and Technology, University of Twente, Meander 229, P.O. Box 217, 7500 AE Enschede (Netherlands); Dukstiene, Nijole [Department of Physical and Inorganic Chemistry, Kaunas University of Technology, Radvilenu pl. 19, LT-50254 Kaunas (Lithuania); Roberts, Adam [Kratos Analytical Ltd, Trafford Wharf Road, Wharfside, Manchester, M17 1GP (United Kingdom); Fairley, Neal [Casa Software Ltd, Bay House, 5 Grosvenor Terrace, Teignmouth, Devon TQ14 8NE (United Kingdom)

    2015-01-30

    Highlights: • We analyzed and modeled spectral envelopes of complex molybdenum oxides. • Molybdenum oxide films of varying valence and crystallinity were synthesized. • MoO{sub 3} and MoO{sub 2} line shapes from experimental data were created. • Informed amorphous sample model (IASM) developed. • Amorphous molybdenum oxide XPS envelopes were interpreted. - Abstract: Accurate elemental oxidation state determination for the outer surface of a complex material is of crucial importance in many science and engineering disciplines, including chemistry, fundamental and applied surface science, catalysis, semiconductors and many others. X-ray photoelectron spectroscopy (XPS) is the primary tool used for this purpose. The spectral data obtained, however, is often very complex and can be subject to incorrect interpretation. Unlike traditional XPS spectra fitting procedures using purely synthetic spectral components, here we develop and present an XPS data processing method based on vector analysis that allows creating XPS spectral components by incorporating key information, obtained experimentally. XPS spectral data, obtained from series of molybdenum oxide samples with varying oxidation states and degree of crystallinity, were processed using this method and the corresponding oxidation states present, as well as their relative distribution was elucidated. It was shown that monitoring the evolution of the chemistry and crystal structure of a molybdenum oxide sample due to an invasive X-ray probe could be used to infer solutions to complex spectral envelopes.

  17. Investigation of the CANLUB/sheath interface in CANDU fuel at extended burnup by XPS and SEM/WDX

    International Nuclear Information System (INIS)

    Hocking, W.H.; Behnke, R.; Duclos, A.M.; Gerwing, A.F.; Chan, P.K.

    1997-01-01

    A systematic investigation of the fuel-sheath interface in CANDU fuel as a function of extended burnup has been undertaken by XPS and SEM/WDX analysis. Adherent deposits of UO 2 and fission products, including Cs, Ba, Rb, I, Te, Cd and possibly Ru, have been routinely identified on CANLUB coated and bare Zircaloy surfaces. Some trends in the distribution and chemistry of key fission products have begun to emerge. Several potential mechanisms for degradation of the CANLUB graphite layer at high burnup have been practically excluded. New evidence of carbon relocation within the fuel element and limited reaction with excess oxygen has also been obtained. (author)

  18. An Auger and XPS survey of cerium active corrosion protection for AA2024-T3 aluminum alloy

    Energy Technology Data Exchange (ETDEWEB)

    Uhart, A. [IPREM-ECP-UMR CNRS 5254, Université de Pau et des Pays de l' Adour, Technopole Hélioparc, 2 Avenue Président Pierre Angot, 64053 Pau Cedex 09 (France); Ledeuil, J.B. [IPREM-ECP-UMR CNRS 5254, Université de Pau et des Pays de l' Adour, Technopole Hélioparc, 2 Avenue Président Pierre Angot, 64053 Pau Cedex 09 (France); Université de Toulouse, UPS-INP-CNRS, Institut Carnot CIRIMAT, 118 Route de Narbonne, 31062 Toulouse Cedex 09 (France); Gonbeau, D. [IPREM-ECP-UMR CNRS 5254, Université de Pau et des Pays de l' Adour, Technopole Hélioparc, 2 Avenue Président Pierre Angot, 64053 Pau Cedex 09 (France); Dupin, J.C., E-mail: dupin@univ-pau.fr [IPREM-ECP-UMR CNRS 5254, Université de Pau et des Pays de l' Adour, Technopole Hélioparc, 2 Avenue Président Pierre Angot, 64053 Pau Cedex 09 (France); Bonino, J.P.; Ansart, F. [Université de Toulouse, UPS-INP-CNRS, Institut Carnot CIRIMAT, 118 Route de Narbonne, 31062 Toulouse Cedex 09 (France); Esteban, J. [Messier-Bugatti-Dowty, Etablissement de Molsheim, 3, rue Antoine de St Exupéry, 67129 Molsheim (France)

    2016-12-30

    Graphical abstract: Coupled SAM/SEM survey of cerium inhibitor migration towards corrosion pits in a conversion coating over AA2024-T3 substrate. - Highlights: • XPS evidenced the proximity of the inhibitor with the surface AA2024 alloy. • Cerium conversion coatings with [Ce] = 0.1 M offer the best corrosion resistance. • SAM shown the migration of Ce + III entities towards the corrosion pits or crevices. • High resolution analyses (Auger) connecting the nano-scale order with the chemical distribution.

  19. XPS investigations of ruthenium deposited onto representative inner surfaces of nuclear reactor containment buildings

    Energy Technology Data Exchange (ETDEWEB)

    Mun, C. [Institut de Radioprotection et de Surete Nucleaire (IRSN), Direction de la Prevention des Accidents Majeurs (DPAM), Centre de Cadarache, BP3-13115 Saint-Paul-lez-Durance (France)]. E-mail: christian.mun@irsn.fr; Ehrhardt, J.J. [Laboratoire de Chimie Physique et Microbiologie pour l' Environnement (LCPME) UMR 7564, CNRS-Nancy University-405, rue de Vandoeuvre 54600 Villers-les-Nancy (France)]. E-mail: ehrhardt@lcpe.cnrs-nancy.fr; Lambert, J. [Laboratoire de Chimie Physique et Microbiologie pour l' Environnement (LCPME) UMR 7564, CNRS-Nancy University-405, rue de Vandoeuvre 54600 Villers-les-Nancy (France); Madic, C. [Commissariat a l' Energie Atomique (CEA), Direction de l' Energie Nucleaire, Centre de Saclay, 91191 Gif-sur-Yvette Cedex (France)]. E-mail: charles.madic@cea.fr

    2007-07-15

    In the case of a hypothetical severe accident in a nuclear power plant, interactions of gaseous RuO{sub 4} with reactor containment building surfaces (stainless steel and epoxy paint) could possibly lead to a black Ru-containing deposit on these surfaces. Some scenarios include the possibility of formation of highly radiotoxic RuO{sub 4}(g) by the interactions of these deposits with the oxidizing medium induced by air radiolysis, in the reactor containment building, and consequently dispersion of this species. Therefore, the accurate determination of the chemical nature of ruthenium in the deposits is of the high importance for safety studies. An experiment was designed to model the interactions of RuO{sub 4}(g) with samples of stainless steel and of steel covered with epoxy paint. Then, these deposits have been carefully characterised by scanning electron microscopy (SEM/EDS), electron probe microanalysis (EPMA) and X-ray photoelectron spectroscopy (XPS). The analysis by XPS of Ru deposits formed by interaction of RuO{sub 4}(g), revealed that the ruthenium is likely to be in the IV oxidation state, as the shapes of the Ru 3d core levels are very similar with those observed on the RuO{sub 2}.xH{sub 2}O reference powder sample. The analysis of O 1s peaks indicates a large component attributed to the hydroxyl functional groups. From these results, it was concluded that Ru was present on the surface of the deposits as an oxyhydroxide of Ru(IV). It has also to be pointed out that the presence of 'pure' RuO{sub 2}, or of a thin layer of RuO{sub 3} or Ru{sub 2}O{sub 5}, coming from the decomposition of RuO{sub 4} on the surface of samples of stainless steel and epoxy paint, could be ruled out. These findings will be used for further investigations of the possible revolatilisation phenomena induced by ozone.

  20. Interaction of cysteine and copper ions on the surface of iron: EIS, polarization and XPS study

    International Nuclear Information System (INIS)

    El-Deab, Mohamed S.

    2011-01-01

    Highlights: → The current study demonstrates a comprehensive study for Cysteine + Cu(II) ions as an efficient inhibitor as demonstrated by EIS, XPS and potentiodynamic polarization measurements, in addition to traditional weight loss measurements. → The novelty of the current work originates from the combined use of an eco-friendly compound (i.e., cysteine) with a minute amount of copper ions (in the micro molar range) as a corrosion inhibitor for low carbon steel in acidic medium. To this end, cysteine shows only moderate inhibition ca. 60% for iron which jumps up to more than 95% in the presence of micro molar range of Cu(II) ions. → Cysteine-Cu(II) blends are found superior to benzotriazole (BTAH)-Cu(II) blends in terms of their long-term stability in addition to the avoidance of the use of the well-reported highly toxic BTAH. - Abstract: This study addresses the enhancing effect of copper ions on the inhibition efficiency (IE) of cysteine (an eco-friendly compound) against the corrosion of iron in 0.5 M sulphuric acid. Electrochemical impedance spectroscopy (EIS) data revealed a significant increase in the polarization resistance (R p ) of the iron/solution interface in the presence of cysteine and Cu(II) ions instead of cysteine alone. That is, IE of 95% is obtained in the presence of 5 mM cysteine and 25 μM Cu(II) ions, compared to 66% in absence of Cu(II) ions. Moreover, electrochemical polarization measurements indicate that cysteine and Cu(II) ions blends act as mixed-type inhibitors for the corrosion of iron. The formation of Cu(I)-cysteinate complex and/or cysteine SAM at Cu atop the iron surface (as evident from X-ray photoelectron spectroscopy (XPS)) blocks the underlying iron surface and imparts a pronounced protection against its corrosion. IE of cysteine-Cu(II) blend remains effectively unchanged with immersion time indicating its high stability in the used acidic medium.

  1. An XPS study of pulsed plasma polymerised allyl alcohol film growth on polyurethane

    Energy Technology Data Exchange (ETDEWEB)

    Watkins, Lucy [Department of Chemistry, University of York, Heslington, York YO10 5DD (United Kingdom); Bismarck, Alexander [Department of Chemical Engineering, Polymer and Composite Engineering (PaCE) Group, Imperial College London, London SW7 2AZ (United Kingdom); Lee, Adam F. [Department of Chemistry, University of York, Heslington, York YO10 5DD (United Kingdom); Wilson, Darren [Smith and Nephew Research Centre, York Science Park, Heslington, York YO10 5DF (United Kingdom); Wilson, Karen [Department of Chemistry, University of York, Heslington, York YO10 5DD (United Kingdom)]. E-mail: kw13@york.ac.uk

    2006-09-30

    The growth of highly functionalised poly allyl alcohol films by pulsed plasma polymerisation of CH{sub 2} =CHCH{sub 2}OH on biomedical grade polyurethane has been followed by X-ray photoelectron spectroscopy (XPS) and contact angle measurements. Film thickness is observed to increase approximately linearly with plasma modification time, suggesting a layer-by-layer growth mode of poly allyl alcohol. Water contact angle measurements reveal the change in the surface free energy of wetting decreases linearly with plasma modification up to the monolayer point after which a constant limiting value of -24 mJ m{sup -2} was attained. Films prepared at 20 W plasma power with a duty cycle of 10 {mu}s:500 {mu}s exhibit a high degree of hydroxyl (-OH) retention with minimal fragmentation of the monomer observed. Increasing the plasma power up to 125 W is found to improve -OH retention at the expense of ether formation generating films close to the monomer stoichiometry. Duty cycle plays an important role in controlling both film composition and thickness, with longer off times increasing -OH retention, while longer on times enhance allyl alcohol film growth.

  2. 13C NMR and XPS characterization of anion adsorbent with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse

    Science.gov (United States)

    Cao, Wei; Wang, Zhenqian; Zeng, Qingling; Shen, Chunhua

    2016-12-01

    Despite amino groups modified crop straw has been intensively studied as new and low-cost adsorbent for removal of anionic species from water, there is still a lack of clear characterization for amino groups, especially quaternary ammonium groups in the surface of crop straw. In this study, we used 13C NMR and XPS technologies to characterize adsorbents with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse. 13C NMR spectra clearly showed the presence of quaternary ammonium groups in lignocelluloses structure of modified crop straw. The increase of nitrogen observed in XPS survey spectra also indicated the existence of quaternary ammonium group in the surface of the adsorbents. The curve fitting of high-resolution XPS N1s and C1s spectra were conducted to probe the composition of nitrogen and carbon contained groups, respectively. The results showed the proportion of quaternary ammonium group significantly increased in the prepared adsorbent's surface that was dominated by methyl/methylene, hydroxyl, quaternary ammonium, ether and carbonyl groups. This study proved that 13C NMR and XPS could be successfully utilized for characterization of quaternary ammonium modified crop straw adsorbents.

  3. Synchrotron-radiation XPS analysis of ultra-thin silane films: Specifying the organic silicon

    Energy Technology Data Exchange (ETDEWEB)

    Dietrich, Paul M., E-mail: paul.dietrich@yahoo.de [Bundesanstalt für Materialforschung und – prüfung (BAM), Unter den Eichen 87, 12205 Berlin (Germany); Glamsch, Stephan [Bundesanstalt für Materialforschung und – prüfung (BAM), Unter den Eichen 87, 12205 Berlin (Germany); Freie Universität Berlin, Institut für Chemie und Biochemie, Fabeckstr. 34/36, 14195 Berlin (Germany); Ehlert, Christopher [Bundesanstalt für Materialforschung und – prüfung (BAM), Unter den Eichen 87, 12205 Berlin (Germany); Institut für Chemie, Universität Potsdam, Karl-Liebknecht-Straße 24-25, 14476 Potsdam (Germany); Lippitz, Andreas [Bundesanstalt für Materialforschung und – prüfung (BAM), Unter den Eichen 87, 12205 Berlin (Germany); Kulak, Nora [Freie Universität Berlin, Institut für Chemie und Biochemie, Fabeckstr. 34/36, 14195 Berlin (Germany); Unger, Wolfgang E.S. [Bundesanstalt für Materialforschung und – prüfung (BAM), Unter den Eichen 87, 12205 Berlin (Germany)

    2016-02-15

    Graphical abstract: - Highlights: • A synchrotron-based XPS method to analyze ultra-thin silane films is presented. • Specification and quantification of organic next to inorganic silicon is demonstrated. • Non-destructive chemical depth profiles of the silane monolayers were obtained. - Abstract: The analysis of chemical and elemental in-depth variations in ultra-thin organic layers with thicknesses below 5 nm is very challenging. Energy- and angle-resolved XPS (ER/AR-XPS) opens up the possibility for non-destructive chemical ultra-shallow depth profiling of the outermost surface layer of ultra-thin organic films due to its exceptional surface sensitivity. For common organic materials a reliable chemical in-depth analysis with a lower limit of the XPS information depth z{sub 95} of about 1 nm can be performed. As a proof-of-principle example with relevance for industrial applications the ER/AR-XPS analysis of different organic monolayers made of amino- or benzamidosilane molecules on silicon oxide surfaces is presented. It is demonstrated how to use the Si 2p core-level region to non-destructively depth-profile the organic (silane monolayer) – inorganic (SiO{sub 2}/Si) interface and how to quantify Si species, ranging from elemental silicon over native silicon oxide to the silane itself. The main advantage of the applied ER/AR-XPS method is the improved specification of organic from inorganic silicon components in Si 2p core-level spectra with exceptional low uncertainties compared to conventional laboratory XPS.

  4. Versatile technique for assessing thickness of 2D layered materials by XPS

    Science.gov (United States)

    Zemlyanov, Dmitry Y.; Jespersen, Michael; Zakharov, Dmitry N.; Hu, Jianjun; Paul, Rajib; Kumar, Anurag; Pacley, Shanee; Glavin, Nicholas; Saenz, David; Smith, Kyle C.; Fisher, Timothy S.; Voevodin, Andrey A.

    2018-03-01

    X-ray photoelectron spectroscopy (XPS) has been utilized as a versatile method for thickness characterization of various two-dimensional (2D) films. Accurate thickness can be measured simultaneously while acquiring XPS data for chemical characterization of 2D films having thickness up to approximately 10 nm. For validating the developed technique, thicknesses of few-layer graphene (FLG), MoS2 and amorphous boron nitride (a-BN) layer, produced by microwave plasma chemical vapor deposition (MPCVD), plasma enhanced chemical vapor deposition (PECVD), and pulsed laser deposition (PLD) respectively, were accurately measured. The intensity ratio between photoemission peaks recorded for the films (C 1s, Mo 3d, B 1s) and the substrates (Cu 2p, Al 2p, Si 2p) is the primary input parameter for thickness calculation, in addition to the atomic densities of the substrate and the film, and the corresponding electron attenuation length (EAL). The XPS data was used with a proposed model for thickness calculations, which was verified by cross-sectional transmission electron microscope (TEM) measurement of thickness for all the films. The XPS method determines thickness values averaged over an analysis area which is orders of magnitude larger than the typical area in cross-sectional TEM imaging, hence provides an advanced approach for thickness measurement over large areas of 2D materials. The study confirms that the versatile XPS method allows rapid and reliable assessment of the 2D material thickness and this method can facilitate in tailoring growth conditions for producing very thin 2D materials effectively over a large area. Furthermore, the XPS measurement for a typical 2D material is non-destructive and does not require special sample preparation. Therefore, after XPS analysis, exactly the same sample can undergo further processing or utilization.

  5. An XPS study on the attachment of triethoxsilylbutyraldehyde to two titanium surfaces as a way to bond chitosan

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Holly J. [Dave C. Swalm School of Chemical Engineering, James Worth Bagley College of Engineering, Mississippi State University, Box 9595, Mississippi State, MS 39762 (United States)], E-mail: hjp2@msstate.edu; Schulz, Kirk H. [Dave C. Swalm School of Chemical Engineering, James Worth Bagley College of Engineering, Mississippi State University, Box 9595, Mississippi State, MS 39762 (United States); Bumgardner, Joel D. [Department of Biomedical Engineering, Herff College of Engineering, University of Memphis, 330 Engineering Technology Building, Memphis, TN 38152 (United States); Walters, Keisha B. [Dave C. Swalm School of Chemical Engineering, James Worth Bagley College of Engineering, Mississippi State University, Box 9595, Mississippi State, MS 39762 (United States)

    2008-05-30

    A bioactive coating has the ability to create a strong interface between bone tissue and implant. Chitosan, a biopolymer derived from the exoskeletons of shellfish, exhibits many bioactive properties that make it an ideal material for use as a coating such as antibacterial, biodegradable, non-toxic, and the ability to attract and promote bone cell growth and organized bone formation. A previous study reported on the bonding of chitosan to a titanium surface using a three-step process. In the current study, 86.4% de-acetylated chitosan coatings were bound to implant quality titanium in a two-step process that involved the deposition of triethoxsilylbutyraldehyde (TESBA) in toluene, followed by a reaction between the aldehyde of TESBA with chitosan. The chitosan coatings were examined on two different metal treatments to determine if any major differences in the ability of titanium to bind chitosan could be detected. The surface of the titanium metal and the individual reaction steps were examined using X-ray photoelectron spectroscopy (XPS). Following the deposition of TESBA, significant changes were seen in the amounts of oxygen, silicon, carbon, and titanium present on the titanium surface, which were consistent with the anticipated reaction steps. It was demonstrated that more TESBA was bound to the piranha-treated titanium surface as compared to the passivated titanium surface. The two different silane molecules, aminopropyltriethoxysilane (APTES) and TESBA, did not affect the chemistry of the resultant chitosan films. XPS showed that both the formation of unwanted polysiloxanes and the removal of the reactive terminal groups were prevented by using toluene as the carrier solvent to bond TESBA to the titanium surfaces, instead of an aqueous solvent. Qualitatively, the chitosan films demonstrated improved adhesion after using toluene, as the films remained attached to the titanium surface even when placed under the ultra-high vacuum necessary for XPS, unlike the

  6. An XPS study on the attachment of triethoxsilylbutyraldehyde to two titanium surfaces as a way to bond chitosan

    International Nuclear Information System (INIS)

    Martin, Holly J.; Schulz, Kirk H.; Bumgardner, Joel D.; Walters, Keisha B.

    2008-01-01

    A bioactive coating has the ability to create a strong interface between bone tissue and implant. Chitosan, a biopolymer derived from the exoskeletons of shellfish, exhibits many bioactive properties that make it an ideal material for use as a coating such as antibacterial, biodegradable, non-toxic, and the ability to attract and promote bone cell growth and organized bone formation. A previous study reported on the bonding of chitosan to a titanium surface using a three-step process. In the current study, 86.4% de-acetylated chitosan coatings were bound to implant quality titanium in a two-step process that involved the deposition of triethoxsilylbutyraldehyde (TESBA) in toluene, followed by a reaction between the aldehyde of TESBA with chitosan. The chitosan coatings were examined on two different metal treatments to determine if any major differences in the ability of titanium to bind chitosan could be detected. The surface of the titanium metal and the individual reaction steps were examined using X-ray photoelectron spectroscopy (XPS). Following the deposition of TESBA, significant changes were seen in the amounts of oxygen, silicon, carbon, and titanium present on the titanium surface, which were consistent with the anticipated reaction steps. It was demonstrated that more TESBA was bound to the piranha-treated titanium surface as compared to the passivated titanium surface. The two different silane molecules, aminopropyltriethoxysilane (APTES) and TESBA, did not affect the chemistry of the resultant chitosan films. XPS showed that both the formation of unwanted polysiloxanes and the removal of the reactive terminal groups were prevented by using toluene as the carrier solvent to bond TESBA to the titanium surfaces, instead of an aqueous solvent. Qualitatively, the chitosan films demonstrated improved adhesion after using toluene, as the films remained attached to the titanium surface even when placed under the ultra-high vacuum necessary for XPS, unlike the

  7. XPS study of the passive films formed on nitrogen-implanted austenitic stainless steels

    International Nuclear Information System (INIS)

    Marcus, P.; Bussell, M.E.

    1992-01-01

    Austenitic stainless steels (304-type) have been implanted with nitrogen ions in order to investigate the effects of implanted nitrogen on their electrochemical behaviour and on the nature of the passive film formed on the steels in acid (0.5M H 2 SO 4 ). Alloys with two nitrogen doses have been prepared (2.5x10 16 and 2x10 17 N atoms/cm 2 ). The implanted alloys have been characterized by 15 N-NRA (nuclear reaction analysis) and XPS (X-ray photoelectron spectroscopy). Alloy surfaces with well-defined N concentrations were prepared, prior to the electrochemical measurements, by argon-ion sputtering of the implanted material for a fixed time in order to reach a well-defined point on the nitrogen depth profile. The samples were then transferred without exposure to air to an electrochemical cell mounted in an inert gas glove box. The implanted nitrogen modifies the electrochemical behaviour of the alloy. The anodic dissolution in the active state is enhanced, and the current density in the passive state is increased. Surface analysis of the alloys by XPS after passivation shows that implanted nitrogen is enriched on the surface during dissolution and passivation of the alloys. The process by which N is enriched on the surface is anodic segregation, which was first observed and characterized for S on Ni and Ni-Fe alloys. The passive films formed on both the unimplanted and implanted alloys have a bilayer structure with an inner oxide layer and an outer hydroxide layer, but on the nitrogen-implanted alloy, a chromium nitride phase is formed at the expense of the chromium oxide. After passivation of the implanted alloys, three chemical states of nitrogen are detected in the N 1s spectrum. The high binding energy (399.4 eV) peak corresponds to a nitrogen species located on the surface of the passive film, which is produced by reaction of the implanted nitrogen with the solution. (orig./WL)

  8. SEM, Scanning Auger and XPS characterization of chemically pretreated Ti surfaces intended for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Pisarek, M. [Faculty of Materials Science and Engineering, Warsaw University of Technology, Woloska 141, 02-507 Warsaw (Poland); Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw (Poland)], E-mail: marcinp@ichf.edu.pl; Lewandowska, M. [Faculty of Materials Science and Engineering, Warsaw University of Technology, Woloska 141, 02-507 Warsaw (Poland); Roguska, A. [Faculty of Materials Science and Engineering, Warsaw University of Technology, Woloska 141, 02-507 Warsaw (Poland); Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw (Poland); Kurzydlowski, K.J. [Faculty of Materials Science and Engineering, Warsaw University of Technology, Woloska 141, 02-507 Warsaw (Poland); Janik-Czachor, M. [Institute of Physical Chemistry, Polish Academy of Sciences, Kasprzaka 44/52, 01-224 Warsaw (Poland)

    2007-07-15

    Titanium is known as a biocompatible metal characterized by biological and corrosion immunity and good mechanical properties, including a high fracture toughness. In a variety of environments, this metal undergoes 'natural' oxidation which determine its resistance to corrosion. It can also be exposed to chemical treatments in acidic or alkaline solutions which 'enforces' chemical and morphological changes of Ti surface. Those methods, if well controlled, may increase the effective Ti surface area, making it more biocompatible. However, the morphological and chemical factors responsible for their interactions with biological cells are still not well known. The aim of this work was to compare surface chemical and morphological changes introduced by commonly used aqueous NaOH pretreatment with those occurring in a new 'piranha' acidic solution. Particular attention was paid to possible changes which may be decisive for the biocompatibility of the Ti-elements subjected to these surface modifications. Surface analytical techniques such as Auger electron spectroscopy (AES) or X-ray photoelectron spectroscopy (XPS) combined with Ar{sup +} ion sputtering allowed us to investigate in detail the chemical composition of Ti oxide layers. SEM examinations provided morphological characterization of the surface of Ti samples. The results revealed large difference in morphology of Ti surfaces pretreated with different procedures whereas only minor difference in the chemistry of the surfaces were detected.

  9. XPS analysis of PE and EVA samples irradiated at different γ-doses

    Science.gov (United States)

    Dorey, Samuel; Gaston, Fanny; Marque, Sylvain R. A.; Bortolotti, Benjamin; Dupuy, Nathalie

    2018-01-01

    The principal plastic materials used for the fluid contact and storage in the biopharmaceutical industry are mainly made up of semi-crystalline polymers, polyolefins, PVC, Siloxane and PET. The polyethylene (PE) and the polypropylene (PP) are often used as fluid contact in multi-layer materials like films. As one sterilisation way of single-use plastic devices used in medical and pharmaceutical fields can take place via γ-irradiation, the effect of sterilization on plastics must be investigated. The irradiation process leads to the production of radicals, which can generate changes in the polymer structure and on the polymer surface. It is well known that the presence of oxygen with free radicals precede the generation of peroxide species so called ROS (reactive oxygen species) which are highly reactive. The purpose of this work is to investigate the γ-rays impact on the surface of PE (polyethylene) and EVA (polyethylene vinyl alcohol) based films when ionized at different doses. X-ray Photoelectron Spectroscopy (XPS) was applied to determine the surface compositions of the polymers to highlight the different chemical moieties generated during the γ-irradiation process and to monitor the potential presence of the ROS.

  10. Surface science approach to Pt/carbon model catalysts: XPS, STM and microreactor studies

    Science.gov (United States)

    Motin, Abdul Md.; Haunold, Thomas; Bukhtiyarov, Andrey V.; Bera, Abhijit; Rameshan, Christoph; Rupprechter, Günther

    2018-05-01

    Pt nanoparticles supported on carbon are an important technological catalyst. A corresponding model catalyst was prepared by physical vapor deposition (PVD) of Pt on sputtered HOPG (highly oriented pyrolytic graphite). The carbon substrate before and after sputtering as well as the Pt/HOPG system before and after Pt deposition and annealing were examined by XPS and STM. This yielded information on the surface density of defects, which serve as nucleation centres for Pt, and on the size distribution (mean size/height) of the Pt nanoparticles. Two different model catalysts were prepared with mean sizes of 2.0 and 3.6 nm, both turned out to be stable upon UHV-annealing to 300 °C. After transfer into a UHV-compatible flow microreactor and subsequent cleaning in UHV and under mbar pressure, the catalytic activity of the Pt/HOPG model system for ethylene hydrogenation was examined under atmospheric pressure flow conditions. This enabled to determine temperature-dependent conversion rates, turnover frequencies (TOFs) and activation energies. The catalytic results obtained are in line with the characteristics of technological Pt/C, demonstrating the validity of the current surface science based model catalyst approach.

  11. Chemistry Characterization of Jet Aircraft Engine Particulate by XPS: Results from APEX III

    Science.gov (United States)

    Vander Wal, Randy L.; Bryg, Victoria M.

    2014-01-01

    This paper reports XPS analysis of jet exhaust particulate from a B737, Lear, ERJ, and A300 aircraft during the APEX III NASA led field campaign. Carbon hybridization and bonding chemistry are identified by high-resolution scans about the C1s core-shell region. Significant organic content as gauged by the sp3/sp2 ratio is found across engines and platforms. Polar oxygen functional groups include carboxylic, carbonyl and phenol with combined content of 20 percent or more. By lower resolution survey scans various elements including transition metals are identified along with lighter elements such as S, N, and O in the form of oxides. Burning additives within lubricants are probable sources of Na, Ba, Ca, Zn, P and possibly Sn. Elements present and their percentages varied significantly across all engines, not revealing any trend or identifiable cause for the differences, though the origin is likely the same for the same element when observed. This finding suggests that their presence can be used as a tracer for identifying soots from aircraft engines as well as diagnostic for monitoring engine performance and wear.

  12. Surface functional group characterization using chemical derivatization X-ray photoelectron spectroscopy (CD-XPS)

    Energy Technology Data Exchange (ETDEWEB)

    Jagst, Eda

    2011-03-18

    Chemical derivatization - X-ray photolectron spectroscopy (CD-XPS) was applied successfully in order to determine different functional groups on thin film surfaces. Different amino group carrying surfaces, prepared by spin coating, self-assembly and plasma polymerization, were successfully investigated by (XPS) and near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Amino groups were derivatized with the widely used primary amino group tags, pentafluorobenzaldehyde (PFB) and 4-(trifluoromethyl)-benzaldehyde (TFBA), prior to analysis. Primary amino group quantification was then carried out according to the spectroscopical data. Self-assembled monolayers (SAMs) of different terminal groups were prepared and investigated with XPS and spectra were compared with reference surfaces. An angle resolved NEXAFS measurement was applied to determine the orientation of SAMs. Plasma polymerized allylamine samples with different duty cycle, power and pressure values were prepared in order to study the effects of external plasma parameters on the primary amino group retention. CD-XPS was used to quantify the amino groups and experiments show, that the milder plasma conditions promote the retention of amino groups originating from the allylamine monomer. An interlaboratory comparison of OH group determination on plasma surfaces of polypropylene treated with oxygen plasma, was studied. The surfaces were investigated with XPS and the [OH] amount on the surfaces was calculated. (orig.)

  13. Surface modification of pyrolyzed carbon fibres by cyclic voltammetry and their characterization with XPS and dye adsorption

    International Nuclear Information System (INIS)

    Georgiou, P.; Walton, J.; Simitzis, J.

    2010-01-01

    Commercial carbon fibres were pyrolyzed up to 1000 deg. C and were then electrochemically treated by cyclic voltammetry in aqueous electrolyte solutions of H 2 SO 4 , in two potential sweep ranges: a narrow region, N, and a wide region, W, avoiding and including water decomposition, respectively. The anodic and cathodic peaks were correlated with oxide formation and their partial reduction, respectively. The nature of oxygen containing groups on the fibre surfaces was determined by XPS. Wide scan spectra and high energy resolution spectra were recorded through the C 1s, O 1s, N 1s and S 2p photoelectron regions. The ability of the fibres to adsorb methylene blue and alizarin yellow dyes from their aqueous solutions indicates the presence of electron acceptor or donor groups on the fibres, respectively. The carbon fibres were classified into two categories. The first includes electrochemically untreated and treated in the N region, and the second those treated in the W region. The high oxygen concentration and effective dye adsorption on the carbon fibres in the second category indicates that their surfaces were effectively modified. The adsorption of dyes on carbon fibres constitutes a complementary method to XPS for an indirect estimation of oxygen and other groups present on the carbon fibre surfaces.

  14. C:\\Users\\AISA\\Desktop\\A. B. FANDOHAN.xps

    African Journals Online (AJOL)

    AISA

    Lantana camara (verbenaceae) : a potential threat to the effectiveness of ... network was highly suitable for L. camara under current climate. ..... in their historical home range but also because ... environmentally friendly biocontrol protocols.

  15. Direct formation of a polyamide on Ag(111): Joint XPS and STM studies

    Energy Technology Data Exchange (ETDEWEB)

    Schmid, Martin; Steinrueck, Hans-Peter; Gottfried, J. Michael [Lehrstuhl fuer Physikalische Chemie II, Universitaet Erlangen-Nuernberg (Germany); Schmitz, Christoph H.; Ikonomov, Julian; Sokolowski, Moritz [Institut fuer Physikalische und Theoretische Chemie, Universitaet Bonn (Germany)

    2011-07-01

    The polymer poly(p-phenylene terephthalamide) (PPTA) was synthesized on Ag(111) by co-adsorption of the reactive monomer compounds terephthaloyl chloride (TPC) and p-phenylenediamine (PPD) at 300 K. The resulting adsorbate phases were characterised by photoelectron spectroscopy (XPS) and scanning tunneling microscopy (STM). A detailed study of the chemical composition and morphology revealed a complex reaction mechanism, by which the formation of amide bonds leads to folded PPTA polymer chains. According to XPS, the chloride of the TPC precursor is not released as HCl as in the bulk reaction, but remains on the surface as chemisorbed Cl or AgCl. Further temperature-programmed XPS studies of pure TPC on Ag(111) reveal that the molecule decomposes already above 130 K, forming chemisorbed Cl (or AgCl) and a phenylene-dicarbonyl species, which is presumably stabilized by the substrate. The adsorbed chlorine partially desorbs above 800 K as molecular AgCl.

  16. XPS and NEXAFS analysis of dimethyl sulfide adsorbed on the Rh(PVP) nanoparticle surface

    International Nuclear Information System (INIS)

    Niwa, Hironori; Ogawa, Satoshi; Yagi, Shinya; Kutluk, Galif

    2010-01-01

    We have studied the adsorption reaction of dimethyl sulfide (DMS: (CH 3 ) 2 S) on the surface of Rh(PVP) nanoparticles by using AFM, XPS and NEXAFS techniques. The AFM images show the degree of dispersion of the Rh(PVP) nanoparticles depends on the amount of them. The in-situ XPS results indicate that the dissociation reaction of DMS into atomic S does not depend upon the existence of the Rh(PVP) nanoparticles. The NEXAFS results show that there is a strong chemical bonding between Rh(PVP) nanoparticle and atomic S. The ex-situ XPS results show the atomic S adsorbed on the Rh(PVP) nanoparticles partially desorb by exposing to the air. (author)

  17. Upgrade of the Surface Spectrometer at NEPOMUC for PAES, XPS and STM Investigations

    Science.gov (United States)

    Zimnik, S.; Lippert, F.; Hugenschmidt, C.

    2014-04-01

    The characterization of the elemental composition of surfaces is of great importance for the understanding of many surface processes, such as surface segregation or oxidation. Positron-annihilation-induced Auger Electron Spectroscopy (PAES) is a powerful technique for gathering information about the elemental composition of only the topmost atomic layer of a sample. The upgraded surface spectrometer at NEPOMUC (NEtron induced POsitron source MUniCh) enables a comprehensive surface analysis with the complementary techniques STM, XPS and PAES. A new X-ray source for X-ray induced photoelectron spectroscopy (XPS) was installed to gather additional information on oxidation states. A new scanning tunneling microscope (STM) is used as a complementary method to investigate with atomic resolution the surface electron density. The combination of PAES, XPS and STM allows the characterization of both the elemental composition, and the surface topology.

  18. XPS/NEXAFS spectroscopic and conductance studies of glycine on AlGaN/GaN transistor devices

    Science.gov (United States)

    Myers, Matthew; Khir, Farah Liyana Muhammad; Home, Michael A.; Mennell, Christopher; Gillbanks, Jeremy; Tadich, Anton; Baker, Murray V.; Nener, Brett D.; Parish, Giacinta

    2018-03-01

    We report on a study using a combination of XPS/NEXAFS and conductivity measurements to develop a fundamental understanding of how dipolar molecules interact with the heterostructure device surface and affect the device conductivity of AlGaN/GaN heterostructure-based transistors. In such structures, which are increasingly being investigated for chemical and biological sensing, a 2-dimensional electron gas spontaneously forms at the layer interface that is sensitive to the charge characteristics of the exposed surface. Glycine, chosen for this study because it is the simplest of the amino acids and is known to form a zwitterionic configuration when stabilized through intermolecular interactions, was evaporated under ultra-high vacuum conditions onto the device surface and subsequently both XPS/NEXAFS and conductivity measurements were conducted. NEXAFS spectra show a preferential orientation for the Glycine molecules on the surface and evidence for both neutral and zwitterionic species on the surface. In situ conductivity measurements suggest that the negatively charged carboxylate group is closest to the surface. These results are a unique and pivotal contribution to the previous and at times conflicting literature on the zwitterionic nature of Glycine.

  19. XPS Spectra Analysis of Ti2+, Ti3+ Ions and Dye Photodegradation Evaluation of Titania-Silica Mixed Oxide Nanoparticles

    Science.gov (United States)

    Chinh, Vu Duc; Broggi, Alessandra; Di Palma, Luca; Scarsella, Marco; Speranza, Giorgio; Vilardi, Giorgio; Thang, Pham Nam

    2018-04-01

    TiO2-SiO2 mixed oxides have been prepared by the sol-gel technique from tetrabutyl orthotitanate and tetraethyl orthosilicate. The prepared materials were characterized by x-ray diffraction, scanning electron microscopy, energy dispersive x-ray spectroscopy, nitrogen physisorption, Fourier-transform infrared spectroscopy (FT-IR) and x-ray photoelectron spectroscopy (XPS). The results indicate that the TiO2-SiO2 mixed oxides have a large surface area and a nanoscale size. FT-IR spectra show that Ti atoms are bonded to silica by oxygen bridging atoms in Ti-O-Si bonds. The titanium valence states in TiO2-SiO2 mixed oxides were investigated by XPS, and their spectra report the presence of Ti2+ and Ti3+ cations for high silica concentration, suggesting the formation of oxygen vacancies. The photocatalytic activity of the prepared materials has been evaluated for the photodegradation of methylene blue (MB). The mixed oxides were activated by means of a UV light source, and the concentration of MB was monitored by UV-Vis spectroscopy. The synthesized TiO2-SiO2 shows significantly higher MB removal efficiency in comparison with that of the commercial TiO2 Degussa, P25.

  20. Quantitative analysis of satellite structures in XPS spectra of gold and silver

    Energy Technology Data Exchange (ETDEWEB)

    Pauly, N., E-mail: nipauly@ulb.ac.be [Université libre de Bruxelles, Service de Métrologie Nucléaire (CP 165/84), 50 av. F. D. Roosevelt, B-1050 Brussels (Belgium); Yubero, F. [Instituto de Ciencia de Materiales de Sevilla, Univ. Sevilla – CSIC, av. Américo Vespucio 49, E-41092 Sevilla (Spain); Tougaard, S. [Department of Physics, Chemistry and Pharmacy, University of Southern Denmark, DK-5230 Odense M (Denmark)

    2016-10-15

    Highlights: • Accurate determination of the energy loss functions for Au and Ag. • Calculation of effective inelastic electron scattering cross sections for Au and Ag. • Convolution of these cross sections with varying model primary spectra F(E). • Variation of F(E) until a good agreement with experimental XPS spectra is reached. • Quantitative determination of Au 4f and Ag 3d characteristics. - Abstract: Identification of specific chemical states and local electronic environments at surfaces by X-ray photoelectron spectroscopy (XPS) is often difficult because it is not straightforward to quantitatively interpret the shape and intensity of shake-up structures that originate from the photoexcitation process. Indeed the shape and intensity of measured XPS structures are strongly affected by both extrinsic excitations due to electron transport out of the surface and intrinsic excitations induced by the sudden creation of the static core hole. These processes must be taken into account to quantitatively extract, from experimental XPS, the primary excitation spectrum of the considered transition which includes all effects that are part of the initial photo-excitation process, i.e. lifetime broadening, spin–orbit coupling, and multiplet splitting. It was previously shown [N. Pauly, S. Tougaard, F. Yubero, Surf. Sci. 620 (2014) 17] that both extrinsic and intrinsic excitations could be included in an effective energy-differential inelastic electron scattering cross section for XPS which is then convoluted with the primary excitation spectrum to model the full XPS spectrum. This method can thus be applied to determine the primary excitation spectrum from any XPS spectrum. We use this approach in the present paper to determine the Au 4f and Ag 3d photoemission spectra from pure metals. We observe that characteristic energy loss features of the XPS spectra are not only due to photoelectron energy losses. We thus prove the existence of a double shake-up process

  1. A comparative study on defect estimation using XPS and Raman spectroscopy in few layer nanographitic structures.

    Science.gov (United States)

    Ganesan, K; Ghosh, Subrata; Gopala Krishna, Nanda; Ilango, S; Kamruddin, M; Tyagi, A K

    2016-08-10

    Defects in planar and vertically oriented nanographitic structures (NGSs) synthesized by plasma enhanced chemical vapor deposition (PECVD) have been investigated using Raman and X-ray photoelectron spectroscopy. While Raman spectra reveal the dominance of vacancy and boundary type defects respectively in vertical and planar NGSs, XPS provides additional information on vacancy related defect peaks in the C 1s spectrum, which originate from non-conjugated carbon atoms in the hexagonal lattice. Although an excellent correlation prevails between these two techniques, our results show that estimation of surface defects by XPS is more accurate than Raman analysis. Nuances of these techniques are discussed in the context of assessing defects in nanographitic structures.

  2. XPS and SEM studies of chromium oxide films chemically formed on stainless steel 316 L

    International Nuclear Information System (INIS)

    Stefanov, P.; Marinova, T.

    2000-01-01

    The structure and composition of chromium oxide films formed on stainless steel by immersion in a chromium electrolyte have been studied by SEM and XPS. Cr 2 O 3 crystallites in the range 30-150 nm are fully developed and cover the whole surface. The chemical composition in the depth and the thickness of the oxide layer have been determined by XPS sputter profiles. The oxide film can be described within the framework of a double layer consisting of a thin outer hydrated layer and an inner layer of Cr 2 O 3 . (orig.)

  3. Investigating early stages of biocorrosion with XPS: AISI 304 stainless steel exposed to Burkholderia species

    Science.gov (United States)

    Johansson, Leena-Sisko; Saastamoinen, Tuomas

    1999-04-01

    We have investigated the interactions of an exopolymer-producing bacteria, Burkholderia sp. with polished AISI 304 stainless steel substrates using X-ray photoelectron spectroscopy (XPS). Steel coupons were exposed to the pure bacteria culture in a specially designed flowcell for 6 h during which the experiment was monitored in situ with an optical microscope. XPS results verified the formation of biofilm containing extracellular polymer on all the samples exposed to bacteria. Sputter results indicated that some ions needed for metabolic processes were trapped within the biofilm. Changes in the relative Fe concentration and Fe 2p peak shape indicated that also iron had accumulated into the biofilm.

  4. Research on the surface chemical behavior of uranium metal in hydrogen atmosphere by XPS

    International Nuclear Information System (INIS)

    Fu Xiaoguo; Wang Xiaolin; Yu Yong; Zhao Zhengping

    2001-01-01

    The surface chemical behavior clean uranium metal in hydrogen atmosphere at 100 and 200 degree C is studied by X-ray photoelectron spectroscopy (XPS), respectively. It leads to hydriding reaction when the hydrogen exposure is 12.0 Pa·s, and the U4f 7/2 binding energy of UH 3 is found to be 378.7 eV. The higher temperature (200 degree C) is beneficial to UH 3 formation at the same hydrogen exposures. XPS elemental depth profiles indicate that the distribution of uranium surface layer is UO 2 , UH 3 and U after exposure to 174.2 Pa·s hydrogen

  5. Conversion electron Moessbauer and XPS study on the effect of polishing of a stainless steel sample

    International Nuclear Information System (INIS)

    Vertes, Cs.; Kuzmann, E.; Lakatos-Varsanyi, M.; Vertes, A.; Vass, G.; Romhanyi, K.

    1994-01-01

    Conversion electron Moessbauer spectroscopy (CEMS) and XPS has been used for the surface analysis of an 'X10CrNiTi 18/9 (DIN 1.7440)'-type stainless steel in order to determine the supposed structural and/or chemical changes in the surface layer caused by polishing. Both, CEMS and XPS results can be associated with the appearance of Fe nitride in the outer layer of steel samples after polishing, while no sing of nitrogen was detected in the bulk material. (author) 9 refs.; 3 figs.; 1 tab

  6. Thorough XPS analyses on overlithiated manganese spinel cycled around the 3V plateau

    Energy Technology Data Exchange (ETDEWEB)

    Grissa, R. [IPREM ECP − UMR CNRS 5254, Université de Pau et des Pays de l’Adour, Hélioparc Pau-Pyrénées, 2 Avenue du Président Angot, 64053 Pau Cedex 9 (France); Martinez, H., E-mail: herve.martinez@univ-pau.fr [IPREM ECP − UMR CNRS 5254, Université de Pau et des Pays de l’Adour, Hélioparc Pau-Pyrénées, 2 Avenue du Président Angot, 64053 Pau Cedex 9 (France); Cotte, S.; Galipaud, J.; Pecquenard, B. [CNRS, Université de Bordeaux, ICMCB–UPR 9048 and Bordeaux INP, 87 Avenue du Dr. Schweitzer, F-33600 Pessac (France); Cras, F.Le [CEA LETI, 17 rue des Martyrs, F-38054 Grenoble (France); Université Grenoble Alpes, F-38000 Grenoble (France)

    2017-07-31

    Highlights: • Mn2p XPS spectra of Li{sub 1+x}Mn{sub 2-x}O{sub 4} (0 < x < 0.25) fitted with reference samples. • XPS Mn mean oxidation states agrees with XRD structural study. • Li{sub 1.2}Mn{sub 1.8}O{sub 4} thin films cycled versus lithium arounds 3 V in liquid electrolyte. • Electrochemical results (over 20 cycles) related to Mn oxidation states evolution. • Irreversible capacity explained on the basis of XPS by active material delamination. - Abstract: Lithium-rich spinel Li{sub 1.2}Mn{sub 1.8}O{sub 4} thin film electrodes operated at 3 V/Li{sup +}/Li are studied by means of X-ray photoelectron spectroscopy (XPS), mainly on the basis of the evolution of the Mn2p XPS peak during the electrode cycling. The analysis of this core peak has long been debated in literature given its complex character. Based on manganese oxide references, MnO (Mn{sup 2+}), Mn{sub 2}O{sub 3}(Mn{sup 3+}) and Li{sub 2}MnO{sub 3}(Mn{sup 4+}), we propose a deconvolution method to identify each Mn oxidation state. This method is then used for the deconvolution of Mn2p XPS peaks of bulk lithium-rich spinels Li{sub 1+x}Mn{sub 2-x}O{sub 4} (0 ≤ x ≤ 0.25) for validation before proceeding to the study of cycled Li{sub 1.2}Mn{sub 1.8}O{sub 4} thin film electrodes. Electrochemical measurements exhibit significant capacity loss during the first cycle. Based on XPS analyses, this phenomenon could be explained by mechanical breakup of parts of the electrode. A stable behavior during subsequent cycles is then observed. The presence of Mn{sup 2+} species (XPS) at the most top surface of the electrode and the significant polarization observed during the discharge illustrate the kinetical limitation of the two-phase reaction, despite the reduced thickness of the electrode material.

  7. XPS and EELS characterization of Mn{sub 2}SiO{sub 4}, MnSiO{sub 3} and MnAl{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Grosvenor, A.P., E-mail: andrew.grosvenor@usask.ca [Department of Chemistry, University of Saskatchewan, Saskatoon, SK S7N 5C9 (Canada); Bellhouse, E.M., E-mail: erika.bellhouse@arcelormittal.com [Global R & D—Hamilton, ArcelorMittal Dofasco, 1330 Burlington St. E, Hamilton, ON L8N 3J5 (Canada); Korinek, A., E-mail: korinek@mcmaster.ca [Canadian Centre for Electron Microscopy, Brockhouse Institute for Materials Research, McMaster University, 1280 Main St. W., Hamilton, ON L8S 4M1 (Canada); Bugnet, M., E-mail: bugnetm@mcmaster.ca [Canadian Centre for Electron Microscopy, Brockhouse Institute for Materials Research, McMaster University, 1280 Main St. W., Hamilton, ON L8S 4M1 (Canada); McDermid, J.R., E-mail: mcdermid@mcmaster.ca [Steel Research Centre, McMaster University, 1280 Main St. W., Hamilton, ON L8S 4M1 (Canada)

    2016-08-30

    Graphical abstract: XPS and EELS spectra were acquired from Mn2Al2O4, MnSiO3 and Mn2SiO4 standards and unique features identified that will allow unambiguous identification of these compounds when studying the selective oxidation of advanced steels. - Highlights: • Mn2Al2O4, MnSiO3 and Mn2SiO4 standards were synthesized and characterized using both XPS and EELS. • Unique features in both the XPS high resolution and EELS spectra were identified for all compounds. • The spectra can be used to identify these compounds when studying the selective oxidation of steels. - Abstract: X-ray Photoelectron Spectroscopy (XPS) and Electron Energy Loss Spectroscopy (EELS) are strong candidate techniques for characterizing steel surfaces and substrate-coating interfaces when investigating the selective oxidation and reactive wetting of advanced high strength steels (AHSS) during the continuous galvanizing process. However, unambiguous identification of ternary oxides such as Mn{sub 2}SiO{sub 4}, MnSiO{sub 3}, and MnAl{sub 2}O{sub 4} by XPS or EELS, which can play a significant role in substrate reactive wetting, is difficult due to the lack of fully characterized standards in the literature. To resolve this issue, samples of Mn{sub 2}SiO{sub 4}, MnSiO{sub 3} and MnAl{sub 2}O{sub 4} were synthesized and characterized by XPS and EELS. The unique features of the XPS and EELS spectra for the Mn{sub 2}SiO{sub 4}, MnSiO{sub 3} and MnAl{sub 2}O{sub 4} standards were successfully derived, thereby allowing investigators to fully differentiate and identify these oxides at the surface and subsurface of Mn, Si and Al alloyed AHSS using these techniques.

  8. XPS and STEM studies of Allende acid insoluble residues

    Science.gov (United States)

    Housley, R. M.; Clarke, D. R.

    1980-01-01

    Data on Allende acid residues obtained both before and after etching with hot HNO3 are presented. X-ray photoelectron spectra show predominantly carbonaceous material plus Fe-deficient chromite in both cases. The HNO3 oxidizes the carbonaceous material to some extent. The small chromites in these residues have a wide range of compositions somewhat paralleling those observed in larger Allende chromites and in Murchison chromites, especially in the high Al contents; however, they are deficient in divalent cations, which makes them metastable and indicates that they must have formed at relatively low temperatures. It is suggested that they formed by precipitation of Cr(3+) and Fe(3+) from olivine at low temperature or during rapid cooling.

  9. XPS study of the passive layers formed on lead in aqueous nitrate solutions

    International Nuclear Information System (INIS)

    Uchida, Miho; Okuwaki, Akitsugu

    1997-01-01

    The analysis of the lead surface immersed in aqueous nitrate solutions by X-ray photoelectron spectroscopy (XPS) shows the formation of passive oxide layer containing nitrogen compound. The oxide layer formed on the lead surface in aqueous ammonium nitrate solution was hydrolyzed and cracked. (author)

  10. Thermally Annealed Iron (Oxide) Thin Film on an Alumina Barrier Layer, by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Madaan, Nitesh; Kanyal, Supriya S.; Jensen, David S.; Vail, Michael A.; Dadson, Andrew; Engelhard, Mark H.; Linford, Matthew R.

    2013-09-06

    Herein we show characterization of an Fe thin film on Al_2O_3 after thermal annealing under H_2 using Al Ka X-rays. The XPS survey spectrum, narrow Fe 2p scan, and valence band regions are presented. The survey spectrum shows aluminum signals due to exposure of the underlying Al_2O_3 film during Fe nanoparticle formation.

  11. Quantitative depth profiling of K-doped fullerene films using XPS and SIMS

    Czech Academy of Sciences Publication Activity Database

    Oswald, S.; Janda, Pavel; Dunsch, L.

    2003-01-01

    Roč. 141, 1-2 (2003), s. 79-85 E-ISSN 1436-5073 Institutional research plan: CEZ:AV0Z4040901 Keywords : XPS * SIMS * depth profiling * fullerenes * doping Subject RIV: CG - Electrochemistry Impact factor: 0.784, year: 2003

  12. PLA-PMMA blends: A study by XPS and ToF-SIMS

    International Nuclear Information System (INIS)

    Cossement, D.; Gouttebaron, R.; Cornet, V.; Viville, P.; Hecq, M.; Lazzaroni, R.

    2006-01-01

    This paper reports which are the possibilities of quantification by time of flight secondary ion mass spectrometry (ToF-SIMS) for some polymer blends. In order to assess the composition of the mixtures, we studied first different poly(L-lactide)/polymethylmethacrylate (PLA/PMMA) blends by X-ray photoelectron spectroscopy (XPS), this technique being quantitative. By XPS fitting of the C 1s level, we found a very good agreement of the measured concentrations with the initial compositions. Concerning ToF-SIMS data treatment, we used principal component analysis (PCA) on negative spectra allowing to discriminate one polymer from the other one. By partial least square regression (PLS), we found also a good agreement between the ToF-SIMS predicted and initial compositions. This shows that ToF-SIMS, in a similar way to XPS, can lead to quantitative results. In addition, the observed agreement between XPS (60-100 A depth analyzed) and ToF-SIMS (10 A depth analyzed) measurements show that there is no segregation of one of the two polymers onto the surface

  13. Diamond/carbon nanotube composites: Raman, FTIR and XPS spectroscopic studies

    Czech Academy of Sciences Publication Activity Database

    Varga, Marián; Ižák, Tibor; Vretenár, V.; Kozak, Halyna; Holovský, Jakub; Artemenko, Anna; Hulman, M.; Skákalová, V.; Lee, D. S.; Kromka, Alexander

    2016-01-01

    Roč. 111, Jan (2016), s. 54-61 ISSN 0008-6223 R&D Projects: GA ČR GC15-22102J; GA MŠk(CZ) 7AMB14SK037 Institutional support: RVO:68378271 Keywords : diamond * carbon nanotubes * spectroscopy * Raman * FTIR * XPS Subject RIV: JI - Composite Materials Impact factor: 6.337, year: 2016

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lou, Leo [Orthodontic Graduate Program, Faculty of Medicine and Dentistry, University of Alberta (Canada); Nelson, Alan E. [Department of Chemical and Materials Engineering, University of Alberta (Canada)], E-mail: aenelson@dow.com; Heo, Giseon [Department of Statistics, Department of Dentistry, University of Alberta (Canada); Major, Paul W. [Orthodontic Graduate Program, Faculty of Medicine and Dentistry, University of Alberta (Canada)

    2008-08-30

    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.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

    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

  17. XPS and electrochemical studies of the dissolution and passivation of molybdenum-implanted austenitic stainless steels

    International Nuclear Information System (INIS)

    De Vito, E.; Marcus, P.

    1993-01-01

    X-ray Photoelectron Spectroscopy (XPS) was used to investigate the chemical composition and the chemical states of the passive film formed on austenitic stainless steels (Fe-19Cr-10Ni (at.%)) which have been implanted with molybdenum (Mo + , 100 keV, 2.5 x 10 16 at./cm 2 ). Prior to passivation the implanted alloy was characterized by RBS (Rutherford Backscattering Spectroscopy) and XPS. Alloys with well-defined surface concentrations of molybdenum were prepared by ion sputtering the implanted alloy in the preparation chamber of the spectrometer, to a fixed point in the implantation profile. The samples were then transferred without air exposure to a glove box with inert gas in which the electrochemical measurements were performed. After passivation, return transfer of the passivated samples was done with the same transfer device to avoid exposure to air. In 0.5 M H 2 SO 4 , the anodic dissolution current density decreases with increasing Mo content on the alloy surface. Surface analysis by XPS showed that the surface is enriched with molybdenum in the Mo 4+ chemical state. The current density in the passive state is similar for both the non-implanted and the implanted alloys. Surface analysis by XPS showed that the passive film has a bilayer structure (inner oxide and outer hydroxide) and that the hydroxide layer present on the surface of the passive film is markedly enriched with molybdenum in the Mo 6+ chemical state. The XPS measurements indicate that the presence of molybdenum favors the formation of chromium hydroxide at the expense of chromium oxide. A significant enrichment of the alloyed (Cr, Ni) and implanted (Mo) elements was also observed in the metallic phase under the passive film. The possible mechanisms of the effect of molybdenum on the corrosion resistance of stainless steels are discussed in light of the obtained surface analytical results

  18. Morphology and Chemical Composition of soot particles emitted by Wood-burning Cook-Stoves: a HRTEM, XPS and Elastic backscattering Studies.

    Science.gov (United States)

    Carabali-Sandoval, G. A., Sr.; Castro, T.; Peralta, O.; De la Cruz, W.; Días, J.; Amelines, O.; Rivera-Hernández, M.; Varela, A.; Muñoz-Muñoz, F.; Policroniades, R.; Murillo, G.; Moreno, E.

    2014-12-01

    The morphology, microstructure and the chemical composition on surface of soot particles were studied by using high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and elastic backscattering spectrometry. In order to obtain freshly soot particles emitted by home-made wood-burning cook stoves, copper grids for Transmission Electron Microscope (TEM) were placed on the last two of an 8-stages MOUDI cascade impactor. The analysis of HRTEM micrographs revealed the nanostructure and the particle size of soot particles. The XPS survey spectra show a large carbon peak around 285 eV and the oxygen signal at 533 eV. Some differences observed in the carbon/oxygen (C/O) ratio of the particles probably depend on the combustion process efficiency of each cook-stove analyzed. The C-1s XPS spectra show an asymmetric broad peak and other with low intensity that corresponds to sp2 and sp3hybridization, which were fitted with a convolution using Gaussian functions. Elastic backscattering technique allows a chemical elemental analysis of samples and confirms the presence of C, O and Si observed by XPS. Additionally, the morphological properties of soot aggregates were analyzed calculating the border-based fractal dimension (Df). Particles exhibit complex shapes with high values of Df. Also, real-time absorption (σabs) and scattering (σsct) coefficients of fine (with aerodynamic diameter < 2.5 µm) soot particles were measured. The trend in σabs and σsct indicate that the cooking process has two important combustion stages which varied in its flaming strength, being vigorous in the first stage and soft in the second one.

  19. XPS studies of SiO/sub 2/ surface layers formed by oxygen ion implantation into silicon

    Energy Technology Data Exchange (ETDEWEB)

    Schulze, D.; Finster, J. (Karl-Marx-Universitaet, Leipzig (German Democratic Republic). Sektion Chemie); Hensel, E.; Skorupa, W.; Kreissig, U. (Zentralinstitut fuer Kernforschung, Rossendorf bei Dresden (German Democratic Republic))

    1983-03-16

    SiO/sub 2/ surface layers of 160 nm thickness formed by /sup 16/O/sup +/ ion implantation into silicon are examined by X-ray photoelectron spectroscopy measurements into the depth after a step-by-step chemical etching. The chemical nature and the thickness of the transition layer were determined. The results of the XPS measurements show that the outer surface and the bulk of the layers formed by oxygen implantation and subsequent high temperature annealing consist of SiO/sub 2/. There is no evidence for Si or SiO/sub x/ (0

  20. XPS and surface resistivity measurements of plasma - treated FEP co-polymer

    International Nuclear Information System (INIS)

    Pitrus, R.K.; Brack, N.; Liesegang, J.; Pigram, P.J.

    2002-01-01

    Full text: Fluorinated polymers such as fluorinated ethylene propylene (FEP) and poly(tetrafluoroethylene) (PTFE) play an important role in many applications due to their many desirable properties such as chemical resistivity, inertness, electrical stability and low dielectric constant; however, one disadvantage of fluorinated polymers is their extreme surface hydrophobicity. Previous studies show that plasma treatment will modify the surface by increasing the surface free energy and also offer a rapid and convenient method for pre-treating the polymers for many purposes. This paper, through resistivity and XPS (x-ray photoelectron spectroscopy) measurements, attempts to discover basic effects of such plasma treatment. Fluorinated ethylene propylene (FEP) co-polymer film of (0.05) mm thickness (obtained commercially) and with the following structure (CF 2 -CF 2 )-(CF(CF 3 )CF 2 )- was used. A suitable cleaning procedure was used to remove adventitious carbon from the surface. XPS has been used to study FEP film properties. The spectra of XPS were analyzed with the main focus on carbon and fluorine as they compose the elemental component of FEP film. A value of 2.05 was obtained for the F/C ratio, which is slightly higher than the theoretical F/C value estimated from the chemical structure of FEP (F/C 2). The clean film was then air plasma treated (pressure 10 -1 torr and power 30W) for various treatment times to produce a higher energy fluoropolymer surface. XPS studies investigated changes to the polymer surface and determined that oxidation occurs on the FEP surface. The oxidation reactions on the FEP surface form oxygen functional groups such as C-O and C=O groups. The results also show that the percentage of CF 2 and CF 3 in the co-polymer surface decreased with exposure time and the percentage of CF, C-C, C-O and C=O increased. There is a sharp decrease in F/C ratio and increase in O/C ratio. In addition to XPS, the resistivity of FEP-film was measured by a

  1. Comparison of the equivalent width, the autocorrelation width, and the variance as figures of merit for XPS narrow scans

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Bhupinder [Department of Chemistry and Biochemistry, C-100 BNSN, Brigham Young University, Provo, UT 84602 (United States); Velázquez, Daniel; Terry, Jeff [Department of Physics, Illinois Institute of Technology, Chicago, IL 60616 (United States); Linford, Matthew R., E-mail: mrlinford@chem.byu.edu [Department of Chemistry and Biochemistry, C-100 BNSN, Brigham Young University, Provo, UT 84602 (United States)

    2014-12-15

    Highlights: • We apply the equivalent and autocorrelation widths and variance to XPS narrow scans. • This approach is complementary to traditional peak fitting methods. • It is bias free and responsive to subtle chemical changes in spectra. • It has the potential for machine interpretation of spectra and quality control. • It has the potential for analysis of complex spectra and tracking charging/artifacts. - Abstract: X-ray photoelectron spectroscopy (XPS) is widely used in surface and materials laboratories around the world. It is a near surface technique, providing detailed chemical information about samples in the form of survey and narrow scans. To extract the maximum amount of information about materials it is often necessary to peak fit XPS narrow scans. And while indispensable to XPS data analysis, even experienced practitioners can struggle with their peak fitting. In our previous publication, we introduced the equivalent width (EW{sub XPS}) as both a possible machine automated method, one that requires less expert judgment for characterizing XPS narrow scans, and as an approach that may be well suited for the analysis of complex spectra. The EW{sub XPS} figure of merit was applied to four different data sets. However, as previously noted, other width functions are also regularly employed for analyzing functions. Here we evaluate two other width functions for XPS narrow scan analysis: the autocorrelation width (AW{sub XPS}) and the variance (σ{sub XPS}{sup 2}). These widths were applied to the same four sets of spectra studied before: (a) four C 1s narrow scans of ozone-treated carbon nanotubes (CNTs) (EW{sub XPS}: ∼2.11–2.16 eV, AW{sub XPS}: ∼3.9–4.1 eV, σ{sub XPS}{sup 2}: ∼5.0–5.2 eV, and a modified form of σ{sub XPS}{sup 2}, denoted σ{sub XPS}{sup 2*}: ∼6.3–6.8 eV), (b) silicon wafers with different oxide thicknesses (EW{sub XPS}: ∼1.5–2.9 eV, AW{sub XPS}: ∼2.28–4.9, and σ{sub XPS}{sup 2}: ∼0.7–4.9 eV), (iii

  2. Redox-active triazatruxene-based conjugated microporous polymers for high-performance supercapacitors† †Electronic supplementary information (ESI) available: Synthetic procedures and characterization data for all new compounds; general experimental method; thermogravimetry curves; PXRD patterns; SEM and TEM images; XPS spectra. See DOI: 10.1039/c6sc05532j Click here for additional data file.

    Science.gov (United States)

    Li, Xiang-Chun; Zhang, Yizhou; Wang, Chun-Yu; Wan, Yi

    2017-01-01

    Conjugated polymers (CPs) have been intensively explored for various optoelectronic applications in the last few decades. Nevertheless, CP based electrochemical energy storage devices such as supercapacitors remain largely unexplored. This is mainly owing to the low specific capacitance, poor structural/electrochemical stability, and low energy density of most existing CPs. In this contribution, a novel set of redox-active conjugated microporous polymers, TAT-CMP-1 and TAT-CMP-2, based on nitrogen-rich and highly conductive triazatruxene building blocks, were successfully designed and synthesized to explore their potential application as efficient and stable electrode materials for supercapacitors. Despite a moderate surface area of 88 m2 g–1 for TAT-CMP-1 and 106 m2 g–1 for TAT-CMP-2, exceptional specific capacitances of 141 F g–1 and 183 F g–1 were achieved at a current density of 1 A g–1. The resulting polymers exhibited unusually high areal specific capacitance (>160 μF cm–2), which is attributed to the pseudocapacitance resulting from redox-active structures with high nitrogen content. More importantly, the TAT-CMP-2 electrode exhibits excellent cycling stability: only 5% capacitance fading is observed after 10 000 cycles at a high current density of 10 A g–1, enabling the possible use of these materials as electrodes in electrochemical devices. PMID:28451362

  3. Chemical state analysis of conversion coatings by SR-XPS and TEY-XANES

    CERN Document Server

    Noro, H; Nagoshi, M

    2002-01-01

    Chromate coatings on galvanized steel have been studied by Synchrotron Radiation (SR) based techniques that include X-ray Photoelectron Spectroscopy (XPS) and Total-Electron-Yield X-ray Absorption Near Edge Structure (TEY-XANES). Non-destructive depth profiling of the coatings by SR-XPS reveals the enhancement of Cr sup 6 sup + in the outer surface. TEY-XANES spectroscopy based on simple specimen current measurement is demonstrated as an effective technique for analyzing chemical states of conversion coatings on general bulk substrates. The sampling depth of this technique, which exceeds several tens of nanometer, is determined by the penetration length of Auger electrons excited by X-ray and the inelastic mean free path of secondary electrons excited by inelastically scattered Auger electrons. The chemical states of phosphoric acid added chromate coatings are studied using this technique. The phosphoric acid is taken into the chromate coatings as partially changed into zinc and chromium phosphates, and the r...

  4. Detergency of stainless steel surface soiled with human brain homogenate: an XPS study

    Energy Technology Data Exchange (ETDEWEB)

    Richard, M. [Ecole Centrale de Lyon, UMR 5513 LTDS, 69 134 Ecully (France) and Laboratoires ANIOS, 59 260 Lille-Hellemmes (France)]. E-mail: marlene.richard@ec-lyon.fr; Le Mogne, Th. [Ecole Centrale de Lyon, UMR 5513 LTDS, 69 134 Ecully (France); Perret-Liaudet, A. [Hopital Neurologique de Lyon et INSERM U512, 69 394 Lyon (France); Rauwel, G. [Laboratoires ANIOS, 59 260 Lille-Hellemmes (France); Criquelion, J. [Laboratoires ANIOS, 59 260 Lille-Hellemmes (France); De Barros, M.I. [Ecole Centrale de Lyon, UMR 5513 LTDS, 69 134 Ecully (France); Cetre, J.C. [Unite d' Hygiene et d' Epidemiologie, Hopital de la Croix Rousse, 69 317 Lyon (France); Martin, J.M. [Ecole Centrale de Lyon, UMR 5513 LTDS, 69 134 Ecully (France)

    2005-02-15

    In the detergency field of re-usable medical devices, a special attention is focused on the non conventional transmissible agent called prions which is a proteinaceous infectious agent. Few cleaning procedures are effective against prions and few techniques are available to study cleaning effectiveness with respect to proteins in general. In our study, X-ray photoelectron spectroscopy (XPS) has been used to evaluate the effectiveness of detergent formulations to remove proteins from stainless steel surface soiled with a brain homogenate (BH) from human origin. Our results showed that XPS is a reliable surface analysis technique to study chemical species remaining on surface and substrate properties after cleaning procedures. A semi-quantitative evaluation of the detergency effectiveness could also be performed.

  5. SEM and XPS study of layer-by-layer deposited polypyrrole thin films

    Science.gov (United States)

    Pigois-Landureau, E.; Nicolau, Y. F.; Delamar, M.

    1996-01-01

    Layer-by-layer deposition of thin films (a few nm) of polypyrrole was carried out on various substrates such as silver, platinum, electrochemically oxidized aluminum and pretreated glass. SEM micrographs showed that the deposited layers nucleate by an island-type mechanism on hydrated alumina and KOH-pretreated (hydrophilic) glass before forming a continuous film. However, continuous thin films are obtained on chromic acid pretreated (hydrophobic) glass and sputtered Ag or Pt on glass after only 3-4 deposition cycles. The mean deposition rate evaluated by XPS for the first deposition cycles on Ag and Pt is 3 and 4 nm/cycle, respectively, in agreement with previous gravimetric determinations on thicker films, proving the constancy of the deposition rate. The XPS study of the very thin films obtained by a few deposition cycles shows that the first polypyrrole layers are dedoped by hydroxydic (basic) substrate surfaces.

  6. SEM and XPS study of layer-by-layer deposited polypyrrole thin films

    International Nuclear Information System (INIS)

    Pigois-Landureau, E.; Nicolau, Y.F.; Delamar, M.

    1996-01-01

    Layer-by-layer deposition of thin films (a few nm) of polypyrrole was carried out on various substrates such as silver, platinum, electrochemically oxidized aluminum and pretreated glass. SEM micrographs showed that the deposited layers nucleate by an island-type mechanism on hydrated alumina and KOH-pretreated (hydrophilic) glass before forming a continuous film. However, continuous thin films are obtained on chromic acid pretreated (hydrophobic) glass and sputtered Ag or Pt on glass after only 3 endash 4 deposition cycles. The mean deposition rate evaluated by XPS for the first deposition cycles on Ag and Pt is 3 and 4 nm/cycle, respectively, in agreement with previous gravimetric determinations on thicker films, proving the constancy of the deposition rate. The XPS study of the very thin films obtained by a few deposition cycles shows that the first polypyrrole layers are dedoped by hydroxydic (basic) substrate surfaces. copyright 1996 American Institute of Physics

  7. APS- and XPS-investigations of vanadium, vanadium carbide and graphite

    Energy Technology Data Exchange (ETDEWEB)

    Bradshaw, A M; Krause, U [Technische Univ. Muenchen (F.R. Germany). Inst. fuer Physikalische Chemie und Theoretische Chemie

    1975-11-01

    Soft X-ray appearance potential spectroscopy (APS) and X-ray photoelectron spectroscopy (XPS) have been used to study vanadium, vanadium carbide, and graphite. The chemical shifts for vanadium carbide with respect to metallic vanadium and graphite are compared for the two methods. The Csub(K) structure in APS and the valence band in XPS for vanadium carbide show good agreement with the band structure calculations of Neckel and co-workers. Using the band structure calculations of Painter et al. it is also shown how the multi-peak structure in the APS spectrum of graphite is possibly due to density of states effects. It would therefore appear that plasmon coupling plays only a minor role.

  8. Detergency of stainless steel surface soiled with human brain homogenate: an XPS study

    International Nuclear Information System (INIS)

    Richard, M.; Le Mogne, Th.; Perret-Liaudet, A.; Rauwel, G.; Criquelion, J.; De Barros, M.I.; Cetre, J.C.; Martin, J.M.

    2005-01-01

    In the detergency field of re-usable medical devices, a special attention is focused on the non conventional transmissible agent called prions which is a proteinaceous infectious agent. Few cleaning procedures are effective against prions and few techniques are available to study cleaning effectiveness with respect to proteins in general. In our study, X-ray photoelectron spectroscopy (XPS) has been used to evaluate the effectiveness of detergent formulations to remove proteins from stainless steel surface soiled with a brain homogenate (BH) from human origin. Our results showed that XPS is a reliable surface analysis technique to study chemical species remaining on surface and substrate properties after cleaning procedures. A semi-quantitative evaluation of the detergency effectiveness could also be performed

  9. XPS characterization of the anodic oxide film formed on uranium metal in sodium hydroxide solution

    International Nuclear Information System (INIS)

    Fu Xiaoguo; Wang Xiaolin; Guo Huanjun; Wang Qingfu; Zhao Zhengping; Zhong Yongqiang

    2002-01-01

    X-ray photoelectron spectroscopy (XPS) is used to examine the anodic oxide film formed on uranium metal in 0.8 mol/L NaOH solution. The U4f 7/2 fitting spectra suggests that the anodic oxide film is composed of uranium trioxide and a small amount of UO 2+x . Under UHV condition, the U4f peak shifts to the lower binding energy, while a gradual increase in the intensity of U5f peak and the broad of U4f peak are also observed. All of these changes are due to reduction of uranium trioxide in the anodic oxide film. XPS quantitative analysis confirms the occurrence of reduction reaction

  10. Comparison of optical models and signals from XPS and VASE characterized titanium after PBS immersion

    Czech Academy of Sciences Publication Activity Database

    Penttinen, N.; Hasoň, Stanislav; Silvennoinen, M.; Joska, L.; Silvennoinen, R.

    2012-01-01

    Roč. 285, č. 6 (2012), s. 965-968 ISSN 0030-4018 Grant - others:GA ČR(CZ) GAP108/10/1782 Program:GA Institutional research plan: CEZ:AV0Z50040507; CEZ:AV0Z50040702 Keywords : permittivity * XPS titanium * diffractive optical element-based sensor Subject RIV: BO - Biophysics Impact factor: 1.438, year: 2012

  11. XPS investigations on the UV-laser ablation mechanism of poly(ether imide)

    Energy Technology Data Exchange (ETDEWEB)

    Wambach, J; Kunz, T; Schnyder, B; Koetz, R; Wokaun, A [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1999-08-01

    UV-Laser ablated samples of poly(ether imide) [Kapton{sup TM}] were studied with small-spot XPS. Applying fluences above the threshold level (0.167 J/cm{sup 2}) resulted in the expected behaviour of a decline of both nitrogen and oxygen. Below the threshold level a hint for an altered ablation mechanism was found. (author) 1 fig., 5 refs.

  12. Study of the local structure of binary surfaces by electron diffraction (XPS, LEED)

    OpenAIRE

    Gereová, Katarína

    2006-01-01

    Study of local structure of binary surface with usage of ultra-thin film of cerium deposited on a Pd (111) single-crystal surface is presented. X-ray photoelectron spectroscopy and diffraction (XPS, XPD), angle resolved UV photoemission spectroscopy (ARUPS) and low energy electron diffraction (LEED) was used for our investigations. LEED and X-ray excited photoemission intensities results represent a surface-geometrical structure. As well, mapping of ultra-violet photoelectron intensities as a...

  13. Investigation of CoPd alloys by XPS and EPES using the pattern recognition method

    Czech Academy of Sciences Publication Activity Database

    Lesiak, B.; Zemek, Josef; Jiříček, Petr; Jozwik, A.

    2007-01-01

    Roč. 428, - (2007), s. 190-196 ISSN 0925-8388 R&D Projects: GA ČR GA202/06/0459 Institutional research plan: CEZ:AV0Z10100521 Keywords : CoPd alloys * x-ray photoelectron spectroscopy (XPS) * elastic peak electron spectroscopy (EPES) * pattern recognition method * fuzzy k-nearest neighbour rule (fkNN) * quantitative analysis * surface segregation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.455, year: 2007

  14. Lead-silicate glass surface sputtered by an argon cluster ion beam investigated by XPS

    Czech Academy of Sciences Publication Activity Database

    Zemek, Josef; Jiříček, Petr; Houdková, Jana; Jurek, Karel; Gedeon, O.

    2017-01-01

    Roč. 469, Aug (2017), s. 1-6 ISSN 0022-3093 R&D Projects: GA MŠk LM2015088; GA ČR(CZ) GA15-12580S Institutional support: RVO:68378271 Keywords : lead-silicate glass * XPS * BO * NBO * Argon duster ion beam sputtering * X-ray irradiation Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 2.124, year: 2016

  15. An XPS study of tarnishing of a gold mask from a pre-Columbian culture

    International Nuclear Information System (INIS)

    Bastidas, D.M.; Cano, E.; Gonzalez, A.G.; Fajardo, S.; Lleras-Perez, R.; Campo-Montero, E.; Belzunce-Varela, F.J.; Bastidas, J.M.

    2008-01-01

    The tarnishing originated on a hammered gold mask was analysed. Red tarnishing was observed after three years of storage in an indoor environment in the Gold Museum of Banco de la Republica, Bogota, Colombia. Silver sulphide (Ag 2 S) and silver sulphate (Ag 2 SO 4 ) compounds were identified as the origin of the tarnishing phenomenon, which is attributed to environmental contamination. Atomic absorption spectroscopy (AAS) and X-ray photoelectron spectroscopy (XPS) techniques were used

  16. Formation of titanium nitride layers on titanium metal: Results of XPS and AES investigations

    International Nuclear Information System (INIS)

    Moers, H.; Pfennig, G.; Klewe-Nebenius, H.; Penzhorn, R.D.; Sirch, M.; Willin, E.

    1988-09-01

    The reaction of titanium metal with gaseous nitrogen and ammonia at temperatures of 890 0 C leads to the formation of nitridic overlayers on the metallic substrate. The thicknesses of the overlayers increase with increasing reaction time. Under comparable conditions ammonia reacts much slower than nitrogen. XPS and AES depth profile analyses show continuous changes of the in-depth compositions of the overlayers. This can be interpreted in terms of a very irregular thickness of the overlayers, an assumption which is substantiated by local AES analyses and by the observation of a pronounced crystalline structure of the substrate after annealing pretreatment, which can give rise to locally different reaction rates. The depth profile is also influenced by the broad ranges of stability of the titanium nitride phases formed during the reaction. The quantitative analysis of the titanium/nitrogen overlayers by AES is difficult because of the overlap of titanium and nitrogen Auger peaks. In quantitative XPS analysis problems arise due to difficulties in defining Ti 2p peak areas. This work presents practical procedures for the quantitative evaluation by XPS and AES of nitridic overlayers with sufficient accuracy. (orig.) [de

  17. Gold/silver core-shell 20 nm nanoparticles extracted from citrate solution examined by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Engelhard, Mark H.; Smith, Jordan N.; Baer, Donald R.

    2016-06-01

    Silver nanoparticles of many types are widely used in consumer and medical products. The surface chemistry of particles and the coatings that form during synthesis or use in many types of media can significantly impact the behaviors of particles including dissolution, transformation and biological or environmental impact. Consequently it is useful to be able to extract information about the thickness of surface coatings and other attributes of nanoparticles produced in a variety of ways. It has been demonstrated that X-ray Photoelectron Spectroscopy (XPS) can be reliably used to determine the thickness of organic and other nanoparticles coatings and shells. However, care is required to produce reliable and consistent information. Here we report the XPS spectra from gold/silver core-shell nanoparticles of nominal size 20 nm removed from a citrate saturated solution after one and two washing cycles. The Simulation of Electron Spectra for Surface Analysis (SESSA) program had been used to model peak amplitudes to obtain information on citrate coatings that remain after washing and demonstrate the presence of the gold core. This data is provided so that others can compare use of SESSA or other modeling approaches to quantify the nature of coatings to those already published and to explore the impacts particle non-uniformities on XPS signals from core-shell nanoparticles.

  18. GD-OES and XPS coupling: A new way for the chemical profiling of photovoltaic absorbers

    Energy Technology Data Exchange (ETDEWEB)

    Mercier, Dimitri, E-mail: dimitri.mercier@uvsq.fr [Institut Lavoisier de Versailles, 45 av. des Etats-Unis, 78035 Versailles Cedex (France); Bouttemy, Muriel; Vigneron, Jackie [Institut Lavoisier de Versailles, 45 av. des Etats-Unis, 78035 Versailles Cedex (France); Chapon, Patrick [HORIBA Jobin Yvon SAS, F-91165 Longjumeau (France); Etcheberry, Arnaud [Institut Lavoisier de Versailles, 45 av. des Etats-Unis, 78035 Versailles Cedex (France)

    2015-08-30

    Highlights: • The coupling between GD-OES and XPS analysis is a promising way for fine characterization of thin layers. • Crater surface modifications obtained after GD-OES sputtering depend to the plasma gas. • Inversion of the gas flow improves the surface of the crater. • The modified layer is totally eliminated a few seconds after restarting GD-OES sputtering. - Abstract: In this paper, we examine the complementarity of Glow Discharge Optical Emission Spectroscopy (GD-OES) and X Ray Photoelectron Spectroscopy (XPS) for the realization of fine chemical depth profiling of photovoltaic absorbers using Cu(In,Ga)Se{sub 2} (CIGS) materials. The possibility to use sequentially these two techniques is discussed in this paper. We have evaluated the chemical modifications of the crater after GD-OES analyses which depend on the manner of finishing the plasma etching sequence; and we propose different ways to limit or eliminate this effect. For the moment, an intermediate step (wet chemical etching or weak sputtering) is required to obtain a CIGS phase in the crater. Finally, we have demonstrated the possibility to restart the GD-OES analyses of the materials after XPS quantification or GD-OES breaking without modifying the profile shape.

  19. Morphological, chemical and structural characterisation of deciduous enamel: SEM, EDS, XRD, FTIR and XPS analysis.

    Science.gov (United States)

    Zamudio-Ortega, C M; Contreras-Bulnes, R; Scougall-Vilchis, R J; Morales-Luckie, R A; Olea-Mejía, O F; Rodríguez-Vilchis, L E

    2014-09-01

    The purpose of this study was to characterise the enamel surface of sound deciduous teeth in terms of morphology, chemical composition, structure and crystalline phases. The enamel of 30 human deciduous teeth was examined by: Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). Chemical differences between incisors and canines were statistically evaluated using the Mann-Whitney U test (p ≤ 0.05). Three enamel patterns were observed by SEM: 'mostly smooth with some groves', 'abundant microporosities' and 'exposed prisms'. The average Ca/P molar ratios were 1.37 and 1.03 by EDS and XPS, respectively. The crystallite size determined by XRD was 210.82 ± 16.78 Å. The mean ratio between Ca bonded to phosphate and Ca bonded to hydroxyl was approximately 10:1. The enamel of sound deciduous teeth showed two main patterns: 'mostly smooth with some groves' and 'abundant microporosities'. 'Exposed prisms' was a secondary pattern. There were slight variations among the Ca/P molar ratios found by EDS and XPS, suggesting differences in the mineral content from the enamel surface to the interior. The crystalline phases found in enamel were hydroxyapatite and carbonate apatite, with major type B than type A carbonate incorporation.

  20. Surface chemical characterization of PM{sub 10} samples by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Atzei, Davide, E-mail: datzei@unica.it [Dipartimento di Scienze Chimiche e Geologiche, Università di Cagliari, Complesso Universitario di Monserrato, S.S. 554 Bivio per Sestu, I-09042 Monserrato, Cagliari (Italy); Fantauzzi, Marzia; Rossi, Antonella [Dipartimento di Scienze Chimiche e Geologiche, Università di Cagliari, Complesso Universitario di Monserrato, S.S. 554 Bivio per Sestu, I-09042 Monserrato, Cagliari (Italy); Fermo, Paola [Dipartimento di Chimica, Università degli Studi Milano, Via Golgi 19, I-20133 Milano (Italy); Piazzalunga, Andrea [Dipartimento di Chimica, Università degli Studi Milano, Via Golgi 19, I-20133 Milano (Italy); Dipartimento di Scienze dell’Ambiente e del territorio, Università degli Studi di Milano-Bicocca, Piazza della Scienza 1, I-20122 Milano (Italy); Valli, Gianluigi; Vecchi, Roberta [Dipartimento di Fisica, Università degli Studi di Milano, via Celoria 16, I-20133 Milano (Italy)

    2014-07-01

    Samples of particulate matter (PM) collected in the city of Milan during wintertime were analyzed by X-ray photoelectron spectroscopy (XPS), thermal optical transmittance (TOT), ionic chromatography (IC) and X-ray fluorescence (XRF) in order to compare quantitative bulk analysis and surface analysis. In particular, the analysis of surface carbon is here presented following a new approach for the C1s curve fitting aiming this work to prove the capability of XPS to discriminate among elemental carbon (EC) and organic carbon (OC) and to quantify the carbon-based compounds that might be present in the PM. Since surface of urban PM is found to be rich in carbon it is important to be able to distinguish between the different species. XPS results indicate that aromatic and aliphatic species are adsorbed on the PM surface. Higher concentrations of (EC) are present in the bulk. Also nitrogen and sulfur were detected on the surfaces and a qualitative and quantitative analysis is provided. Surface concentration of sulfate ion is equal to that found by bulk analysis; moreover surface analysis shows an additional signal due to organic sulfur not detectable by the other methods. Surface appears to be also enriched in nitrogen.

  1. Quantitative Surface Analysis by Xps (X-Ray Photoelectron Spectroscopy: Application to Hydrotreating Catalysts

    Directory of Open Access Journals (Sweden)

    Beccat P.

    1999-07-01

    Full Text Available XPS is an ideal technique to provide the chemical composition of the extreme surface of solid materials, vastly applied to the study of catalysts. In this article, we will show that a quantitative approach, based upon fundamental expression of the XPS signal, has enabled us to obtain a consistent set of response factors for the elements of the periodic table. In-depth spadework has been necessary to know precisely the transmission function of the spectrometer used at IFP. The set of response factors obtained enables to perform, on a routine basis, a quantitative analysis with approximately 20% relative accuracy, which is quite acceptable for an analysis of such a nature. While using this quantitative approach, we have developed an analytical method specific to hydrotreating catalysts that allows obtaining the sulphiding degree of molybdenum quite reliably and reproducibly. The usage of this method is illustrated by two examples for which XPS spectroscopy has provided with information sufficiently accurate and quantitative to help understand the reactivity differences between certain MoS2/Al2O3 or NiMoS/Al2O3-type hydrotreating catalysts.

  2. XPS and EPXMA investigation and chemical speciation of aerosol samples formed in LWR core melting experiments

    International Nuclear Information System (INIS)

    Moers, H.; Jenett, H.; Kaufmann, R.; Klewe-Nebenius, H.; Pfennig, G.; Ache, H.J.

    1985-09-01

    Aerosol samples consisting of fission products and elements of light water reactor structural materials were collected during simulating in a laboratory scale the heat-up phase of a core melt accident. The aerosol particles were formed in a steam atmosphere at temperatures between 1200 and 1900 0 C of the melting charge. The investigation of the samples by use of X-ray photoelectron spectroscopy (XPS) permitted the chemical speciation of the detected aerosol constituents silver, cadmium, indium, tellurium, iodine, and cesium. A comparison of the elemental analysis results obtained from XPS with those achieved from electron probe X-ray micro analysis (EPXMA) revealed that aerosol particle surface and aerosol particle bulk are principally composed of the same elements and that these compositions vary with release temperature. In addition, quantitative differences between the composition of surface and bulk have only been observed for those aerosol samples which were collected at higher melting charge temperatures. In order to obtain direct information on chemical species below the surface selected samples were argon ion bombarded. Changes in composition and chemistry were monitored by XPS, and the results were interpreted in light of the effects, which were observed when appropriate standard samples were sputtered. (orig.) [de

  3. XPS and NEXAFS study of tyrosine-terminated propanethiol assembled on gold

    CERN Document Server

    Petoral, R M

    2003-01-01

    Tyrosine-terminated propanethiol (TPT), tyrosine linked to 3-mercaptopropionic acid through an amide bond, is adsorbed to gold surfaces. The adsorbates are characterized by means of X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure spectroscopy (NEXAFS). XPS is used to investigate the chemical binding and electronic structure of the monolayer. Strong molecular binding of the tyrosine derivative on the gold surface through the sulfur atom is attained. Angle-dependent XPS results shows that TPT molecules are oriented with the sulfur atoms molecularly oriented close to the gold surface and that the phenol moiety is oriented away from the gold surface. Average orientation of the adsorbate on gold is deduced using the NEXAFS results. It shows that the main molecular axis is tilted approximately 38 deg. relative to the Au surface normal. The ring plane of the phenol moiety exhibits a preferential orientation with an average tilt angle of the normal of the ring plane from the surfa...

  4. XPS investigations of tribolayers formed on TiN and (Ti,Re)N coatings

    Energy Technology Data Exchange (ETDEWEB)

    Oktay, Serkan; Kahraman, Zafer; Urgen, Mustafa; Kazmanli, Kursat, E-mail: kursat@itu.edu.tr

    2015-02-15

    Graphical abstract: - Highlights: • The (Ti,Re)N coating (8 ± 1.9 at.% Re) consisted of TiN and ReNx (x > 1.33) phases. • TiO{sub 2} provided low friction coefficient to TiN coating at 150 °C. • Re addition to TiN drastically dropped the friction coefficients to 0.17–0.22. • Re{sub 2}O{sub 7} provided very low friction coefficient to (Ti,Re)N coating. • Re addition to TiN improved the wear behavior. - Abstract: TiN and (Ti,Re)N coatings were deposited on high-speed-steel substrates by a hybrid coating system composed of cathodic arc PVD and magnetron sputtering techniques. In order to keep rhenium content low (8 ± 1.9 at.%) in the coating, magnetron sputtering technique was utilized to evaporate rhenium. The (Ti,Re)N coating consisted of TiN and ReN{sub x} (x > 1.33) phases. The hardness of TiN and (Ti,Re)N were 31 GPa and 29 GPa ( ± 2 GPa), respectively. Tribological behaviors of the samples were tested against Al{sub 2}O{sub 3} balls at 21 °C (RT) and 150 °C (HT) by reciprocating wear technique. The tribolayers were analyzed by XPS technique. Friction coefficients of TiN were 0.56, 0.35 for 21 °C and 150 °C tests, respectively. Rhenium addition to TiN drastically dropped the friction coefficients to 0.22 and 0.17 for RT and HT samples. Rhenium addition also improved the wear resistance of the coating at both test temperatures. For TiN, main oxide component of the tribolayers was Ti{sub 2}O{sub 3} for RT tests and TiO{sub 2} for HT tests. The oxide layer formed on (Ti,Re)N were the mixture of TiO{sub 2}, Ti−O−N, ReO{sub 2} and Re{sub 2}O{sub 7} for both test temperatures. Re{sub 2}O{sub 7} provided very low friction coefficient to (Ti,Re)N. The findings are consistent with the crystal chemistry approach.

  5. Cohort study comparing prostate photovaporisation with XPS 180W and HPS 120W laser.

    Science.gov (United States)

    López, B; Capitán, C; Hernández, V; de la Peña, E; Jiménez-Valladolid, I; Guijarro, A; Pérez-Fernández, E; Llorente, C

    2016-01-01

    Prostate photovaporisation with Greenlight laser for the surgical treatment of benign prostate hyperplasia has rapidly evolve to the new XPS 180W. We have previously demonstrated the safety and efficacy of the HPS 120W. The aim of this study was to assess the functional and safety results, with a year of follow-up, of photovaporisation using the XPS 180W laser compared with its predecessor. A cohort study was conducted with a series of 191 consecutive patients who underwent photovaporisation between 1/2008 and 5/2013. The inclusion criteria were an international prostate symptom score (IPSS) >15 after medical failure, a prostate volume <80 cm(3) and a maximum flow <15 mL/s. We assessed preoperative and intraoperative variables (energy used, laser time and total surgical time), complications, catheter hours, length of stay and functional results (maximum flow, IPSS, prostate-specific antigen and prostate volume) at 3, 6 and 12 months. We analysed the homogeneity in preoperative characteristics of the 2 groups through univariate analysis techniques. The postoperative functional results were assessed through an analysis of variance of repeated measures with mixed models. A total of 109 (57.1%) procedures were performed using HPS 120W, and 82 (42.9%) were performed using XPS. There were no differences between the preoperative characteristics. We observed significant differences both in the surgical time and effective laser time in favour of the XPS system. This advantage was 11% (48 ± 15.7 vs. 53.8 ± 16.2, p<.05) and 9% (32.8 ± 11.7 vs. 36 ± 11.6, p<.05), respectively. There were no statistically significant differences in the rest of the analysed parameters. The technical improvements in the XPS 180W system help reduce surgical time, maintaining the safety and efficacy profile offered by the HPS 120W system, with completely superimposable results at 1 year of follow-up. Copyright © 2015 AEU. Publicado por Elsevier España, S.L.U. All rights reserved.

  6. In Situ Studies of Surface Mobility on Noble Metal Model Catalysts Using STM and XPS at Ambient Pressure

    Energy Technology Data Exchange (ETDEWEB)

    Butcher, Derek Robert [Univ. of California, Berkeley, CA (United States)

    2010-06-01

    High Pressure Scanning Tunneling Microscopy (HP-STM) and Ambient Pressure X-ray Photoelectron Spectroscopy were used to study the structural properties and catalytic behavior of noble metal surfaces at high pressure. HP-STM was used to study the structural rearrangement of the top most atomic surface layer of the metal surfaces in response to changes in gas pressure and reactive conditions. AP-XPS was applied to single crystal and nanoparticle systems to monitor changes in the chemical composition of the surface layer in response to changing gas conditions. STM studies on the Pt(100) crystal face showed the lifting of the Pt(100)-hex surface reconstruction in the presence of CO, H2, and Benzene. The gas adsorption and subsequent charge transfer relieves the surface strain caused by the low coordination number of the (100) surface atoms allowing the formation of a (1 x 1) surface structure commensurate with the bulk terminated crystal structure. The surface phase change causes a transformation of the surface layer from hexagonal packing geometry to a four-fold symmetric surface which is rich in atomic defects. Lifting the hex reconstruction at room temperature resulted in a surface structure decorated with 2-3 nm Pt adatom islands with a high density of step edge sites. Annealing the surface at a modest temperature (150 C) in the presence of a high pressure of CO or H2 increased the surface diffusion of the Pt atoms causing the adatom islands to aggregate reducing the surface concentration of low coordination defect sites. Ethylene hydrogenation was studied on the Pt(100) surface using HP-STM. At low pressure, the lifting of the hex reconstruction was observed in the STM images. Increasing the ethylene pressure to 1 Torr, was found to regenerate the hexagonally symmetric reconstructed phase. At room temperature ethylene undergoes a structural rearrangement to form ethylidyne. Ethylidyne preferentially binds at the three-fold hollow sites, which

  7. X-ray photoemission spectroscopy (XPS) study of uranium, neptunium and plutonium oxides in silicate-based glasses

    International Nuclear Information System (INIS)

    Lam, D.J.; Veal, B.W.; Paulikas, A.P.

    1982-11-01

    Using XPS as the principal investigative tool, we are in the process of examining the bonding properties of selected metal oxides added to silicate glass. In this paper, we present results of XPS studies of uranium, neptunium, and plutonium in binary and multicomponent silicate-based glasses. Models are proposed to account for the very diverse bonding properties of 6+ and 4+ actinide ions in the glasses

  8. Al2O3 e-Beam Evaporated onto Silicon (100)/SiO2, by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Madaan, Nitesh; Kanyal, Supriya S.; Jensen, David S.; Vail, Michael A.; Dadson, Andrew; Engelhard, Mark H.; Samha, Hussein; Linford, Matthew R.

    2013-09-25

    We report the XPS characterization of a thin film of Al2O3 (35 nm) deposited via e-beam evaporation onto silicon (100). The film was characterized with monochromatic Al Ka radiation. An XPS survey scan, an Al 2p narrow scan, and the valence band spectrum were collected. The Al2O3 thin film is used as a diffusion barrier layer for templated carbon nanotube (CNT) growth in the preparation of microfabricated thin layer chromatography plates.

  9. Effects of Mn Ion Implantation on XPS Spectroscopy of GaN Thin Films

    Science.gov (United States)

    Majid, Abdul; Ahmad, Naeem; Rizwan, Muhammad; Khan, Salah Ud-Din; Ali, Fekri Abdulraqeb Ahmed; Zhu, Jianjun

    2018-02-01

    Gallium nitride (GaN) thin film was deposited onto a sapphire substrate and then implanted with 250 keV Mn ions at two different doses of 2 × 1016 ions/cm2 and 5 × 1016 ions/cm2. The as-grown and post-implantation-thermally-annealed samples were studied in detail using x-ray photoelectron spectroscopy (XPS). The XPS peaks of Ga 3 d, Ga 2 p, N 1 s, Mn 2 p and C 1 s were recorded in addition to a full survey of the samples. The doublet peaks of Ga 2 p for pure GaN were observed blue-shifted when compared with elemental Ga, and appeared further shifted to higher energies for the implanted samples. These observations point to changes in the bonds and the chemical environment of the host as a result of ion implantation. The results revealed broadening of the N 1 s peak after implantation, which is interpreted in terms of the presence of N-Mn bonds in addition to N-Ga bonds. The XPS spectra of Mn 2 p recorded for ion-implanted samples indicated splitting of Mn 2 p 1/2 and Mn 2 p 3/2 peaks higher than that for metallic Mn, which helps rule out the possibility of clustering and points to substitutional doping of Mn. These observations provide a framework that sheds light on the local environment of the material for understanding the mechanism of magnetic exchange interactions in Mn:GaN based diluted magnetic semiconductors.

  10. XNAES and XPS studies on modification of SWCNTS upon gas-phase purification treatments

    International Nuclear Information System (INIS)

    Liang Xianqing; Wu Ziyu; Zhong Jun; Zhao Ting; Yao Peng; Ibrahim, K.; Qian Haijie

    2009-01-01

    A systematic characterization of single-walled carbon nanotubes (SWCNTs) after successive purification steps, including air oxidation at 350 degree C, hydrochloric acid etching and 600 degree C annealing in Ar, have been performed combining X-ray absorption near-edge structure (XANES) and X-ray photoelectron spectroscopy (XPS). The results indicated that the modification degree of SWCNTs increased after the purification procedures, but decreased significantly by annealing in Ar. It also showed that the SWCNTs could bond with chlorine atoms during the hydrochloric acid etching and suggested this modification may be importance for the applications. (authors)

  11. Atomic and nuclear analytical methods. XRF, Moessbauer, XPS, NAA and ion-beam spectroscopic techniques

    International Nuclear Information System (INIS)

    Verma, H.R.

    2007-01-01

    This book is a blend of analytical methods based on the phenomenon of atomic and nuclear physics. It comprises comprehensive presentations about X-ray Fluorescence (XRF), Moessbauer Spectroscopy (MS), X-ray Photoelectron Spectroscopy (XPS), Neutron- Activation Analysis (NAA), Particle Induced X-ray Emission Analysis (PIXE), Rutherford Backscattering Analysis (RBS), Elastic Recoil Detection (ERD), Nuclear Reaction Analysis (NRA), Particle Induced Gamma-ray Emission Analysis (PIGE), and Accelerator Mass Spectrometry (AMS). These techniques are commonly applied in the fields of medicine, biology, environmental studies, archaeology or geology et al. and pursued in major international research laboratories. (orig.)

  12. Combined application of XANES and XPS to study oxygen species adsorbed on Ag foil

    CERN Document Server

    Bukhtiyarov, V I; Kaichev, V V; Knop-Gericke, A; Mayer, R W; Schloegl, R

    2001-01-01

    Adsorbed oxygen species realized in the course of ethylene epoxidation over polycrystalline silver have been characterized by X-ray absorption near the edge structure and X-ray photoelectron spectroscopy. Namely, the combined application of XANES and XPS in similar UHV conditions using the same sample allowed us to assign an XAS feature to the nucleophilic and electrophilic oxygen. This is of great significance, since these species are suggested to be included into the active center for ethylene epoxidation. The differences in the oxygen-silver bonding of these oxygen species are discussed.

  13. Multiwalled Carbon Nanotube Forest Grown via Chemical Vapor Deposition from Iron Catalyst Nanoparticles, by XPS

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, David S.; Kanyal, Supriya S.; Madaan, Nitesh; Vail, Michael A.; Dadson, Andrew; Engelhard, Mark H.; Linford, Matthew R.

    2013-09-25

    Carbon nanotubes (CNTs) have unique chemical and physical properties. Herein, we report an XPS analysis of a forest of multiwalled CNTs using monochromatic Al Kα radiation. Survey scans show only one element: carbon. The carbon 1s peak is centered 284.5 eV. The C 1s envelope also shows the expected π → π* shake-up peak at ca. 291 eV. The valence band and carbon KVV Auger signals are presented. When patterned, the CNT forests can be used as a template for subsequent deposition of metal oxides to make thin layer chromatography plates.1-3

  14. XPS and Raman study of zinc containing silica microparticles loaded with insulin

    Energy Technology Data Exchange (ETDEWEB)

    Vanea, E.; Simon, V., E-mail: viorica.simon@phys.ubbcluj.ro

    2013-09-01

    Zinc–silica microparticles obtained by sol–gel method solely or by combining sol–gel chemistry with freeze-drying and spray-drying procedures were explored as potential insulin drug delivery carriers for their improved loading efficiency. Zinc containing silica hosts of different specific surface area and mean pore volume loaded with insulin under similar conditions were investigated by X-ray photoelectron spectroscopy (XPS) and confocal micro-Raman spectroscopy in order to assess the insulin adherence to these matrices and the biologically active state of the insulin after embedding.

  15. XPS response in the corrosion products analysis for copper exposed at clean air environment

    International Nuclear Information System (INIS)

    Mariaca, L.; Morcillo, M.; Feliu Jr, S.; Gonzalez, J.A.

    1998-01-01

    In this work is presented the obtained response for superficial analysis technique by X-ray photoelectron spectroscopy (XPS or ESCA), to determine the corrosion products formed during the copper exposure at environment without pollutants (clean air) at 50, 70 and 90 % of relative humidity at 35 Centigrade. One of the copper corrosion products most knew is Cu 2 O. This oxide is formed instantly to be exposed the copper at air. However in function of the exposure time and the relative humidity at it is exposed, the Cu 2 O oxide is transformed at Cu O and Cu(OH) 2 (Author)

  16. ISS Assessment of the Influence of Nonpore Surface in the XPS Analysis of Oil-Producing Reservoir Rocks

    Science.gov (United States)

    Leon; Toledo; Araujo

    1997-08-15

    The application of X-ray photoelectron spectroscopy (XPS) to oil-producing reservoir rocks is new and has shown that pore surface concentrations can be related to rock wettability. In the preparation of fresh fractures of rocks, however, some nonpore surface corresponding to the connection regions in the rocks is created and exposed to XPS. To assess the potential influence of this nonpore surface in the XPS analysis of rocks here we use ion scattering spectroscopy (ISS), which has a resolution comparable to the size of the pores, higher than that of XPS, with an ion gun of He+ at maximum focus. Sample charging effects are partially eliminated with a flood gun of low energy electrons. All the ISS signals are identified by means of a formula which corrects any residual charging on the samples. Three rock samples are analyzed by XPS and ISS. The almost unchanged ISS spectra obtained at different points of a given sample suggest that the nonpore surface created in the fracture process is negligibly small, indicating that XPS data, from a larger surface spot, represents the composition of true pore surfaces. The significant changes observed in ISS spectra from different samples indicate that ISS is sample specific. Copyright 1997Academic Press

  17. New insights into micro/nanoscale combined probes (nanoAuger, μXPS) to characterize Ag/Au@SiO2 core-shell assemblies

    Science.gov (United States)

    Ledeuil, J. B.; Uhart, A.; Soulé, S.; Allouche, J.; Dupin, J. C.; Martinez, H.

    2014-09-01

    This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (~12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies.This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming

  18. XPS and μ-Raman study of nanosecond-laser processing of poly(dimethylsiloxane) (PDMS)

    Energy Technology Data Exchange (ETDEWEB)

    Armyanov, S., E-mail: armyanov@ipc.bas.bg [Rostislaw Kaischew Institute of Physical Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., Block 11, Sofia 1113 (Bulgaria); Stankova, N.E.; Atanasov, P.A. [Institute of Electronics, Bulgarian Academy of Sciences, 72 Tsarigradsko Shose, Sofia 1784 (Bulgaria); Valova, E.; Kolev, K.; Georgieva, J. [Rostislaw Kaischew Institute of Physical Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., Block 11, Sofia 1113 (Bulgaria); Steenhaut, O.; Baert, K.; Hubin, A. [Vrije Universiteit Brussels, Faculty of Engineering, Research Group, SURF “Electrochemical and Surface Engineering” (Belgium)

    2015-10-01

    Data about the chemical status of poly(dimethylsiloxane) (PDMS) after nanosecond Q-switched Nd:YAG laser treatment with near infrared, visible and ultraviolet radiation are presented. The μ-Raman spectroscopy analyses reveal as irradiation result a new sharp peak of crystalline silicon. In addition, broad bands appear assigned to D band of amorphous carbon and G band of microcrystalline and polycrystalline graphite. The μ-Raman spectra are variable taken in different inspected points in the trenches formed by laser treatment. The XPS surface survey spectra indicate the constituent elements of PDMS: carbon, oxygen and silicon. The spectra of detail XPS scans illustrate the influence of the laser treatment. The position of Si 2p peaks of the treated samples is close to the value of non-treated except that irradiated by 1064 nm 66 pulses, which is shifted by 0.9 eV. Accordingly, a shift by 0.4 eV is noticed of the O 1s peak, which reflects again a stronger oxidation of silicon. The curve fitting of Si 2p and O 1s peaks after this particular laser treatment shows the degree of conversion of organic to inorganic silicon that takes place during the irradiation.

  19. Spectroellipsometric, AFM and XPS probing of stainless steel surfaces subjected to biological influences

    Science.gov (United States)

    Vinnichenko, M.; Chevolleau, Th; Pham, M. T.; Poperenko, L.; Maitz, M. F.

    2002-11-01

    Surface modification of austenitic stainless steel (SS) 316L after incubation in growing cell cultures and cell-free media as control has been studied. The following treatments were applied: mouse fibrosarcoma cells L929 for 3 and 7 days, polymorphonuclear neutrophils for 3 and 7 days and human osteosarcoma cells SAOS-2 for 7 and 14 days. Cells were enzymatically removed in all cases. The modified surfaces were probed in comparison with untreated ones by means of spectroscopic ellipsometry (SE), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). XPS shows the appearance of the peak of bonded nitrogen at 400.5 eV characteristic for adsorbed proteins on the surface for each type of cells and for the cell-free medium. Migration of Ni in the adsorbed layer is observed in all cases for samples after the cell cultures. The protein layer thickness is ellipsometrically determined to be within 2.5-6.0 nm for all treated samples with parameterization of its optical constants in Cauchy approach. The study showed that for such biological treatments of the SS the protein layer adsorption is the dominating process in the first 2 weeks, which could play a role in the process of corrosion by complex forming properties with metal ions.

  20. Spectroellipsometric, AFM and XPS probing of stainless steel surfaces subjected to biological influences

    International Nuclear Information System (INIS)

    Vinnichenko, M.; Chevolleau, Th.; Pham, M.T.; Poperenko, L.; Maitz, M.F.

    2002-01-01

    Surface modification of austenitic stainless steel (SS) 316L after incubation in growing cell cultures and cell-free media as control has been studied. The following treatments were applied: mouse fibrosarcoma cells L929 for 3 and 7 days, polymorphonuclear neutrophils for 3 and 7 days and human osteosarcoma cells SAOS-2 for 7 and 14 days. Cells were enzymatically removed in all cases. The modified surfaces were probed in comparison with untreated ones by means of spectroscopic ellipsometry (SE), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). XPS shows the appearance of the peak of bonded nitrogen at 400.5 eV characteristic for adsorbed proteins on the surface for each type of cells and for the cell-free medium. Migration of Ni in the adsorbed layer is observed in all cases for samples after the cell cultures. The protein layer thickness is ellipsometrically determined to be within 2.5-6.0 nm for all treated samples with parameterization of its optical constants in Cauchy approach. The study showed that for such biological treatments of the SS the protein layer adsorption is the dominating process in the first 2 weeks, which could play a role in the process of corrosion by complex forming properties with metal ions

  1. Structural, optical, XPS and magnetic properties of Zn particles capped by ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Morozov, Iu.G., E-mail: yugmor@hotmail.com [Institute of Structural Macrokinetics and Materials Science, Russian Academy of Sciences, Academician Osipyan Street 8, Chernogolovka, Moscow Region 142432 (Russian Federation); Belousova, O.V. [Institute of Structural Macrokinetics and Materials Science, Russian Academy of Sciences, Academician Osipyan Street 8, Chernogolovka, Moscow Region 142432 (Russian Federation); Ortega, D., E-mail: daniel.ortega@imdea.org [Instituto Madrileño de Estudios Avanzados en Nanociencia (IMDEA-Nanociencia), Cantoblanco 28049, Madrid (Spain); Mafina, M.-K., E-mail: m.k.mafina@qmul.ac.uk [School of Engineering and Materials Science, Queen Mary University of London, Mile End, Eng, 231, London E1 4NS (United Kingdom); Kuznetcov, M.V., E-mail: maxim1968@mail.ru [Department of Chemistry, Materials Chemistry Research Centre, University College London, 20 Gordon Street, London WC1H 0AJ (United Kingdom)

    2015-06-05

    Highlights: • Levitation-jet aerosol synthesis of Zn particles capped by ZnO nanoparticles (NPs). • TEM, XRD, UV–vis, FT-IR, Raman, XPS and magnetic characterization of the NPs. • Correlation between unit-cell volume of crystal lattice and maximum magnetization. - Abstract: Spherical zinc particles ranging from 42 to 760 nm in average size and capped with plate-like zinc oxide particles of 10–30 nm in sizes have been prepared by levitation-jet aerosol synthesis through condensation of zinc vapor in an inert/oxidizer gas flow. The nanoparticles have been characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), BET measurements, ultra violet visible (UV–vis) spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, X-ray electron spectroscopy (XPS), superconducting quantum interference device (SQUID), and vibrating-sample magnetometer (VSM). Magnetic and XRD data indicate that the observed ferromagnetic ordering related to the changes in unit-cell volume of Zn in the Zn/ZnO interface of the nanoparticles. These results are in good correlation with the optical measurements data.

  2. XPS/STM study of model bimetallic Pd–Au/HOPG catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Bukhtiyarov, Andrey V., E-mail: avb@catalysis.ru [Boreskov Institute of Catalysis, Lavrentieva Ave. 5, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova str. 2, 630090 Novosibirsk (Russian Federation); Prosvirin, Igor P., E-mail: prosvirin@catalysis.ru [Boreskov Institute of Catalysis, Lavrentieva Ave. 5, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova str. 2, 630090 Novosibirsk (Russian Federation); Bukhtiyarov, Valerii I., E-mail: vib@catalysis.ru [Boreskov Institute of Catalysis, Lavrentieva Ave. 5, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova str. 2, 630090 Novosibirsk (Russian Federation)

    2016-03-30

    Graphical abstract: - Highlights: • The model Pd–Au/HOPG catalysts preparation has been studied by XPS and STM. • Model “core–shell” type Pd–Au/HOPG catalysts with different Pd/Au ratios were prepared. • Heating of the “core–shell” Pd–Au/HOPG samples up to 400 °C leads to alloy formation. • Contribution of parameters controlling the properties of Pd–Au alloyed particles has been discussed. - Abstract: The preparation of model bimetallic Pd–Au/HOPG catalysts has been investigated using scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS) techniques. Initially, model “core–shell” type Pd–Au/HOPG catalysts with similar particle size distribution (5–8 nm), but with different densities of particle locations on the HOPG surface and Pd/Au atomic ratios are prepared. Further, their thermal stability is studied within a temperature range of 50–500 °C at UHV conditions. It has been shown that annealing the model catalysts at a temperature range of 300–400 °C leads to formation of Pd–Au alloyed particles. Enhancement of heating temperature up to 500 °C results in sintering of bimetallic nanoparticles. Contribution of different parameters controlling the properties of Pd–Au alloyed particles has been discussed.

  3. The effect of particle-hole interaction on the XPS core-hole spectrum

    International Nuclear Information System (INIS)

    Ohno, Masahide; Sjoegren, Lennart

    2004-01-01

    How the effective particle-hole interaction energy, U, or the polarization effect on a secondary electron in a final two-hole one-particle (2h1p) state created by the Coster-Kronig (CK) transition can solely affect the density of the CK particle states and consequently the core-hole spectral function, is discussed. The X-ray photoelectron spectroscopy (XPS) core-hole spectrum is predominantly governed by the unperturbed initial core-hole energy relative to the zero-point energy. At the latter energy, the real part of the initial core-hole self-energy becomes zero (no relaxation energy shift) and the imaginary part (the lifetime broadening) approximately maximizes. The zero-point energy relative to the double-ionization threshold energy is governed by the ratio of U relative to the bandwidth of the CK continuum. As an example, we study the 5p XPS spectra of atomic Ra (Z=88), Th (Z=90) and U (Z=92). The spectra are interpreted in terms of the change in the unperturbed initial core-hole energy relative to the zero-point energy. We explain why in general an ab initio atomic many-body calculation can provide an overall good description of solid-state spectra predominantly governed by the atomic-like localized core-hole dynamics. We explain this in terms of the change from free atom to metal in both U and the zero-point energy (self-energy)

  4. Rondorfite-type structure — XPS and UV–vis study

    Energy Technology Data Exchange (ETDEWEB)

    Dulski, M., E-mail: mateusz.dulski@smcebi.edu.pl [Institute of Material Science, University of Silesia, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); A.Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Bilewska, K., E-mail: kbilewska@us.edu.pl [A.Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); Institute of Non-Ferrous Metals, Sowińskiego 5, 44-100 Gliwice (Poland); Wojtyniak, M., E-mail: marcin.wojtyniak@us.edu.pl [Institute of Material Science, University of Silesia, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); Szade, J., E-mail: jacek.szade@us.edu.pl [A.Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); Kusz, J., E-mail: joachim.kusz@us.edu.pl [A.Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Nowak, A., E-mail: ana.maria.nowak@gmail.com [A.Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); Wrzalik, R., E-mail: roman.wrzalik@us.edu.pl [A.Chelkowski Institute of Physics, University of Silesia, Uniwersytecka 4, 40-007 Katowice (Poland); Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1a, 41-500 Chorzow (Poland); and others

    2015-10-15

    Highlights: • Structural and spectroscopic characterization of chlorosilicate mineral, rondorfite. • Characterization of main photoemission lines and valence band spectra. • The study of color origin’s using UV–vis spectroscopy. • Analysis of structural changes in context of origin of natural fluorescence. • Discussion of a new application possibilities of analyzed mineral - Abstract: This paper focuses on X-ray diffraction, X-ray photoelectron and UV–vis spectroscopy of two different (green, orange) rondorfite samples. The differences in the sample color originate from various O/Cl ratios. The orange color was found to be related either to the isomorphic substitution of Fe{sup 3+}/Al{sup 3+} for Mg{sup 2+}, the presence of atypical [MgO{sub 4}] tetrahedrons in crystal structure or electronegativity of the sample. The tetrahedron is known to be very prone to accumulation of impurities and substitute atoms. Moreover, the XPS data showed tetrahedrally coordinated Mg{sup 2+} and isomorphic substitution of Al{sup 3+}/Fe{sup 3+} for Mg{sup 2+}, which influences local disordering and the point defects density and distribution. Non-equilibrium chlorine positions inside the crystal cages as well as Ca-Cl bonds have also been found. The XPS measurements as a function of temperature indicate occurrence of a structural transformation at about 770 K which is accompanied by a rotation of silicate tetrahedra within magnesiosilicate pentamer and luminescence disappearance.

  5. XPS analysis of the carbon fibers surface modified via HMDSO to carbon nanotube growth

    Energy Technology Data Exchange (ETDEWEB)

    Cardoso, L.D.R.; Gomes, M.C.B.; Trava-Airoldi, V.J.; Corat, E.J.; Lugo, D.C. [Instituto Nacional de Pesquisas Espaciais (INPE), Sao Jose dos Campos, SP (Brazil)

    2016-07-01

    Full text: Carbon fibers (CF) have been widely used to reinforce structural composites. Due to their strength-to-weight properties, CF composites are finding increased structural uses in areas such as aerospace, aeronautical, automobile and others. The strength of the fiber-resin interface bond has been found to be the limiting factor to the mechanical properties of CF-epoxy materials, due to their non-polar nature that limit the affinity of CF to bind chemically to any matrix. The growth of carbon nanotubes (CNTs) on the surface of CF is a promising approach for improving mechanical, electrical and thermal properties of structural composites. However growing CNTs on CF presents some obstacles, such as diffusion of metal catalyst particles on CF, uneven CNT growth and loss of mechanical properties of CF. To avoid the diffusion of catalyst particles we modified the CF surface with hexamethyldisiloxane (HMDSO) at low temperature (400 °C), also preventing the loss of mechanical properties and allowing uniform CNTs growth. We deposited CNTs via floating catalyst method, with ferrocene providing the catalyst particle and the oxidative dehydrogenation reaction of acetylene providing the carbon. The CF surface modification was analyzed via X-ray photoelectron spectroscopy (XPS) and CNTs growth via scanning electron microscopy with field emission gun. The XPS analysis showed that HMDSO promotes the binding of oxygen to carbon and silicon present on CF surface, the chemical modification of the surface of the CF enables the uniform growth of carbon nanotubes. (author)

  6. Formation of complexes between functionalized chitosan membranes and copper: A study by angle resolved XPS

    Energy Technology Data Exchange (ETDEWEB)

    Jurado-López, Belén [Departamento de Química Inorgánica, Facultad de Ciencias, Universidad de Málaga, 29071 Málaga (Spain); Vieira, Rodrigo Silveira [Chemical Engineering Department, Universidade Federal do Ceará, UFC, 60455-760 Fortaleza, CE (Brazil); Rabelo, Rodrigo Balloni; Beppu, Marisa Masumi [School of Chemical Engineering, University of Campinas, UNICAMP, P.O. Box 6066, 13081-970 Campinas, SP (Brazil); Casado, Juan [Departamento de Química-Física, Facultad de Ciencias, Universidad de Málaga, 29071 Málaga (Spain); Rodríguez-Castellón, Enrique, E-mail: castellon@uma.es [Departamento de Química Inorgánica, Facultad de Ciencias, Universidad de Málaga, 29071 Málaga (Spain)

    2017-01-01

    Chitosan is a biopolymer with potential applications in various fields. Recently, it has been used for heavy metals removal like copper, due to the presence of amino and hydroxyl groups in its structure. Chitosan membranes were crosslinked with epichlorohydrin and bisoxirano and functionalized with chelating agents, such as iminodiacetic acid, aspartic acid and tris-(2-amino-ethyl) polyamine. These membranes were used for copper adsorption and the formed complexes were characterized. Thermal and crystalline properties of chitosan membranes were studied by TG-DCS and X-ray diffraction. Raman, XPS and FT-IR data confirmed that copper is linked to the modified chitosan membranes by the amino groups. The oxidation state of copper-chitosan membranes were also studied by angle resolved XPS, and by UV–Vis diffuse reflectance spectroscopy. - Highlights: • Chitosan membranes were crosslinked with epichlorohydrin and bisoxirano and functionalized with chelating agents. • The chelating agent were iminodiacetic acid, aspartic acid and tris-(2-amino-ethyl) polyamine. • The functionalized membranes were used for copper adsorption and studied by ARXPS, Raman, TG-DCS, FT-IR and XRD. • Spectroscopic data confirmed that copper is linked to the modified chitosan membranes by the amino groups.

  7. XPS analysis of the carbon fibers surface modified via HMDSO to carbon nanotube growth

    International Nuclear Information System (INIS)

    Cardoso, L.D.R.; Gomes, M.C.B.; Trava-Airoldi, V.J.; Corat, E.J.; Lugo, D.C.

    2016-01-01

    Full text: Carbon fibers (CF) have been widely used to reinforce structural composites. Due to their strength-to-weight properties, CF composites are finding increased structural uses in areas such as aerospace, aeronautical, automobile and others. The strength of the fiber-resin interface bond has been found to be the limiting factor to the mechanical properties of CF-epoxy materials, due to their non-polar nature that limit the affinity of CF to bind chemically to any matrix. The growth of carbon nanotubes (CNTs) on the surface of CF is a promising approach for improving mechanical, electrical and thermal properties of structural composites. However growing CNTs on CF presents some obstacles, such as diffusion of metal catalyst particles on CF, uneven CNT growth and loss of mechanical properties of CF. To avoid the diffusion of catalyst particles we modified the CF surface with hexamethyldisiloxane (HMDSO) at low temperature (400 °C), also preventing the loss of mechanical properties and allowing uniform CNTs growth. We deposited CNTs via floating catalyst method, with ferrocene providing the catalyst particle and the oxidative dehydrogenation reaction of acetylene providing the carbon. The CF surface modification was analyzed via X-ray photoelectron spectroscopy (XPS) and CNTs growth via scanning electron microscopy with field emission gun. The XPS analysis showed that HMDSO promotes the binding of oxygen to carbon and silicon present on CF surface, the chemical modification of the surface of the CF enables the uniform growth of carbon nanotubes. (author)

  8. Rotary friction welding of dissimilar joints and bonding interface characterization by EDX and XPS

    Energy Technology Data Exchange (ETDEWEB)

    Alves, Eder Paduan; Dollinger, Christian Avila [Instituto de Aeronautica e Espaco (IAE), Sao Jose dos Campos, SP (Brazil); Marcuzzo, Jossano Saldanha; Baldan, Mauricio Ribeiro; Toledo, Rafael Cardoso; Piorino Neto, Francisco; An, Chen Ying, E-mail: eder.padua@yahoo.com.br [Instituto Nacional de Pesquisas Espaciais (INPE), Sao Jose dos Campos, SP (Brazil)

    2016-07-01

    Full text: Welding of dissimilar materials has been a challenge to engineering. The study and development of new union processes that meet the requirements of projects in the aerospace, nuclear and aviation sector are of great importance to the scientific and productive means. The Rotary friction welding process (RFW) is a process of union that occurs in the solid state, without occurrence of fusion between the parties, and that have like the main bonding mechanisms the diffusion and mechanical mixture. This work has as objective the obtaining of dissimilar joints involving AA 6351-T6 alloy and stainless steel AISI 304l for applications in the aerospace area. The joints obtained by RFW who had procedures and qualified welding process have undergone the techniques of Energy Dispersive X-Ray Spectroscopy (EDX) and X-Ray Photoelectron Spectroscopy (XPS) for analysis of the bonding interface. Were obtained joints with superior mechanical properties the AA 6351-T6 alloy, with the fracture occurring in aluminum away from the bonding interface. The analyses carried out by EDX and XPS have shown the occurrence of interdiffusion among the main elements of the materials involved. The Rotary friction welding process proved to be a great method for obtaining of joints between dissimilar materials that are not possible by fusion welding processes. (author)

  9. Rotary friction welding of dissimilar joints and bonding interface characterization by EDX and XPS

    International Nuclear Information System (INIS)

    Alves, Eder Paduan; Dollinger, Christian Avila; Marcuzzo, Jossano Saldanha; Baldan, Mauricio Ribeiro; Toledo, Rafael Cardoso; Piorino Neto, Francisco; An, Chen Ying

    2016-01-01

    Full text: Welding of dissimilar materials has been a challenge to engineering. The study and development of new union processes that meet the requirements of projects in the aerospace, nuclear and aviation sector are of great importance to the scientific and productive means. The Rotary friction welding process (RFW) is a process of union that occurs in the solid state, without occurrence of fusion between the parties, and that have like the main bonding mechanisms the diffusion and mechanical mixture. This work has as objective the obtaining of dissimilar joints involving AA 6351-T6 alloy and stainless steel AISI 304l for applications in the aerospace area. The joints obtained by RFW who had procedures and qualified welding process have undergone the techniques of Energy Dispersive X-Ray Spectroscopy (EDX) and X-Ray Photoelectron Spectroscopy (XPS) for analysis of the bonding interface. Were obtained joints with superior mechanical properties the AA 6351-T6 alloy, with the fracture occurring in aluminum away from the bonding interface. The analyses carried out by EDX and XPS have shown the occurrence of interdiffusion among the main elements of the materials involved. The Rotary friction welding process proved to be a great method for obtaining of joints between dissimilar materials that are not possible by fusion welding processes. (author)

  10. Incorporation of low energy activated nitrogen onto HOPG surface: Chemical states and thermal stability studies by in-situ XPS and Raman spectroscopy

    Science.gov (United States)

    Chandran, Maneesh; Shasha, Michal; Michaelson, Shaul; Hoffman, Alon

    2016-09-01

    In this paper we report the chemical states analysis of activated nitrogen incorporated highly oriented pyrolytic graphite (HOPG) surface under well-controlled conditions. Nitrogen incorporation is carried out by two different processes: an indirect RF nitrogen plasma and low energy (1 keV) N2+ implantation. Bonding configuration, concentration and thermal stability of the incorporated nitrogen species by aforesaid processes are systematically compared by in-situ X-ray photoelectron spectroscopy (XPS). Relatively large concentration of nitrogen is incorporated onto RF nitride HOPG surface (16.2 at.%), compared to N2+ implanted HOPG surface (7.7 at.%). The evolution of N 1s components (N1, N2, N3) with annealing temperature is comprehensively discussed, which indicates that the formation and reorganization of local chemical bonding states are determined by the process of nitridation and not by the prior chemical conditioning (i.e., amorphization or hydrogenation) of the HOPG surface. A combined XPS and Raman spectroscopy studies revealed that N2+ implantation process resulted in a high level of defects to the HOPG surface, which cannot be annealed-out by heat treatment up to 1000 °C. On the other hand, the RF nitrogen plasma process did not produce a high level of surface defects, while incorporating nearly the same amount of stable nitrogen species.

  11. A XPS Study of the Passivity of Stainless Steels Influenced by Sulfate-Reducing Bacteria.

    Science.gov (United States)

    Chen, Guocun

    The influence of sulfate-reducing bacteria (SRB) on the passivity of type 304 and 317L stainless steels (SS) was investigated by x-ray photoelectron spectroscopy (XPS), microbiological and electrochemical techniques. Samples were exposed to SRB, and then the resultant surfaces were analyzed by XPS, and the corrosion resistance by potentiodynamic polarization in deaerated 0.1 M HCl. To further understand their passivity, the SRB-exposed samples were analyzed by XPS after potentiostatic polarization at a passive potential in the hydrochloric solution. The characterization was performed under two surface conditions: unrinsed and rinsed by deaerated alcohol and deionized water. Comparisons were made with control samples immersed in uninoculated medium. SRB caused a severe loss of the passivity of 304 SS through sulfide formation and possible additional activation to form hexavalent chromium. The sulfides included FeS, FeS_2, Cr_2S _3, NiS and possibly Fe_ {rm 1-x}S. The interaction took place nonuniformly, resulting in undercutting of the passive film and preferential hydration of inner surface layers. The bacterial activation of the Cr^{6+ }^ecies was magnified by subsequent potentiostatic polarization. In contrast, 317L SS exhibited a limited passivity. The sulfides were formed mainly in the outer layers. Although Cr^{6+}^ecies were observed after the exposure, they were dissolved upon polarization. Since 317L SS has a higher Mo content, its higher passivity was ascribed to Mo existing as molybdate on the surface and Mo^{5+} species in the biofilm. Consequently, the interaction of SRB with Mo was studied. It was observed that molybdate could be retained on the surfaces of Mo coupons by corrosion products. In the presence of SRB, however, a considerable portion of the molybdate interacted with intermediate sulfur -containing proteins, forming Mo(V)-S complexes and reducing bacterial growth and sulfate reduction. The limited insolubility of the Mo(V)-S complexes in 0

  12. The Activation of Non-evaporable Getters Monitored by AES, XPS, SSIMS and Secondary Electron Yield Measurements

    CERN Document Server

    Scheuerlein, C

    2002-01-01

    In this thesis the potential of the three classical surface analysis techniques Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) and static secondary ion mass spectrometry (SSIMS) for the characterisation of non-evaporable getter (NEG) materials is assessed and artefacts are described. The various NEG samples have been analysed in the context of the development of NEG thin film coatings for use in accelerator ultra high vacuum (UHV) systems. The secondary electron yield (SEY), which is a functional surface property of great importance for the application of NEG to accelerators, has been measured. The maximum SEY of an air exposed TiZr and TiZrV coating can be reduced from above 2.0 to below 1.1 during a 2 h heat treatment at 250 and 200 °C, respectively. Saturating an activated TiZrV surface in UHV increases the maximum SEY by about 0.1. Thus, in UHV the SEY of an activated NEG coating does not exceed the threshold value of 1.35, above which multipacting is predicted to occur in th...

  13. Oxygen accumulation on metal surfaces investigated by XPS, AES and LEIS, an issue for sputter depth profiling under UHV conditions

    Science.gov (United States)

    Steinberger, R.; Celedón, C. E.; Bruckner, B.; Roth, D.; Duchoslav, J.; Arndt, M.; Kürnsteiner, P.; Steck, T.; Faderl, J.; Riener, C. K.; Angeli, G.; Bauer, P.; Stifter, D.

    2017-07-01

    Depth profiling using surface sensitive analysis methods in combination with sputter ion etching is a common procedure for thorough material investigations, where clean surfaces free of any contamination are essential. Hence, surface analytic studies are mostly performed under ultra-high vacuum (UHV) conditions, but the cleanness of such UHV environments is usually overrated. Consequently, the current study highlights the in principle known impact of the residual gas on metal surfaces (Fe, Mg, Al, Cr and Zn) for various surface analytics methods, like X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and low-energy ion scattering (LEIS). The investigations with modern, state-of-the-art equipment showed different behaviors for the metal surfaces in UHV during acquisition: (i) no impact for Zn, even after long time, (ii) solely adsorption of oxygen for Fe, slight and slow changes for Cr and (iii) adsorption accompanied by oxide formation for Al and Mg. The efficiency of different counter measures was tested and the acquired knowledge was finally used for ZnMgAl coated steel to obtain accurate depth profiles, which exhibited before serious artifacts when data acquisition was performed in an inconsiderate way.

  14. Visualization of Gas Distribution in a Model AP-XPS Reactor by PLIF: CO Oxidation over a Pd(100 Catalyst

    Directory of Open Access Journals (Sweden)

    Jianfeng Zhou

    2017-01-01

    Full Text Available In situ knowledge of the gas phase around a catalyst is essential to make an accurate correlation between the catalytic activity and surface structure in operando studies. Although ambient pressure X-ray photoelectron spectroscopy (AP-XPS can provide information on the gas phase as well as the surface structure of a working catalyst, the gas phase detected has not been spatially resolved to date, thus possibly making it ambiguous to interpret the AP-XPS spectra. In this work, planar laser-induced fluorescence (PLIF is used to visualize the CO2 distribution in a model AP-XPS reactor, during CO oxidation over a Pd(100 catalyst. The results show that the gas composition in the vicinity of the sample measured by PLIF is significantly different from that measured by a conventional mass spectrometer connected to a nozzle positioned just above the sample. In addition, the gas distribution above the catalytic sample has a strong dependence on the gas flow and total chamber pressure. The technique presented has the potential to increase our knowledge of the gas phase in AP-XPS, as well as to optimize the design and operating conditions of in situ AP-XPS reactors for catalysis studies.

  15. Structural and XPS studies of PSi/TiO2 nanocomposites prepared by ALD and Ag-assisted chemical etching

    International Nuclear Information System (INIS)

    Iatsunskyi, Igor; Kempiński, Mateusz; Nowaczyk, Grzegorz; Jancelewicz, Mariusz; Pavlenko, Mykola; Załęski, Karol; Jurga, Stefan

    2015-01-01

    Highlights: • Porous silicon/TiO 2 nanocomposites have been investigated. • Morphology and chemical composition of PSi/TiO 2 nanocomposites were established. • Valence-band XPS maximums for PSi/TiO 2 nanocomposites were found and analyzed. - Abstract: PSi/TiO 2 nanocomposites fabricated by atomic layer deposition (ALD) and metal-assisted chemical etching (MACE) were investigated. The morphology and phase structure of PSi/TiO 2 nanocomposites were studied by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM) with an energy dispersive X-ray spectroscopy (EDX) and Raman spectroscopy. The mean size of TiO 2 nanocrystals was determined by TEM and Raman spectroscopy. X-ray photoelectron spectroscopy (XPS) was used to analyze the chemical elemental composition by observing the behavior of the Ti 2p, O 1s and Si 2p lines. TEM, Raman spectroscopy and XPS binding energy analysis confirmed the formation of TiO 2 anatase phase inside the PSi matrix. The XPS valence band analysis was performed in order to investigate the modification of PSi/TiO 2 nanocomposites electronic structure. Surface defects states of Ti 3+ at PSi/TiO 2 nanocomposites were identified by analyzing of XPS valence band spectra

  16. Study of gadolinia-doped ceria solid electrolyte surface by XPS

    International Nuclear Information System (INIS)

    Datta, Pradyot; Majewski, Peter; Aldinger, Fritz

    2009-01-01

    Gadolinia-doped ceria (CGO) is an important material to be used as electrolyte for solid oxide fuel cell for intermediate temperature operation. Ceria doped with 10 mol% gadolinia (Ce 0.9 Gd 0.1 O 1.95 ) was prepared by conventional solid state synthesis and found to be single phase by room temperature X-ray diffraction (XRD). The chemical states of the surface of the prepared sample were analyzed by X-ray photoelectron spectroscopy (XPS). Though Gd was present in its characteristic chemical state, Ce was found in both Ce 4+ and Ce 3+ states. Presence of Ce 3+ state was ascribed to the differential yield of oxygen atoms in the sputtering process

  17. Corrosion behaviour of Ni in aprotic solvents an electrochemical, XPS and AFM study

    International Nuclear Information System (INIS)

    Bellucci, F.; Monetta, T.; Capobianco, G.; Deganello, A.; Glisenti, A.; Moretti, G.

    1998-01-01

    Electrochemical and X-ray photoelectron spectroscopic (XPS) techniques have been used to study the passivation of nickel in 0.1 M H 2 SO 4 DMF and ACN solutions with different water content. Electrochemical results indicate the anodic formation of a thin, poor protective layer and the possibility of salt precipitation onto the metallic surface. ARXPS results indicate that while in the anodic film formed in DMF, Ni(OH) 2 constitute the superficial component under which a discontinuous layer of NiO and NiSO 4 is present. Ni(OH) 2 and NiSO 4 are the more superficial constituents in the passivation layer formed in ACN, while NiO becomes prevalent in the underlying layers. AFM images show that in both the solvents the sample surface is very dishomogeneous with flakes and fractures. (orig.)

  18. Novel immobilizations of an adhesion peptide on the TiO2 surface: An XPS investigation

    International Nuclear Information System (INIS)

    Iucci, G.; Dettin, M.; Battocchio, C.; Gambaretto, R.; Bello, C. Di; Polzonetti, G.

    2007-01-01

    The covalent attachment of an adhesive peptide, reproducing the 351-359 sequence of human vitronectin, to oxidized titanium surfaces was investigated by XPS spectroscopy. The peptide enhances osteoblast adhesion to titanium, the most used biomaterial for implants and prostheses. Core level spectra of the TiO 2 surface and of the biomimetic surface were investigated. Novel selective covalent immobilization of (351-359) HVP was carried out by treatment of the TiO 2 surface with (3-aminopropyl) triethoxysilane, glutaric anhydride and a side chain protected peptide sequence presenting only a free terminal amino group, followed by side chain deprotection. An alternative strategy for covalent attachment consists in photoactivation of physisorbed (351-359) HVP directly on the TiO 2 surface; samples were incubated with HVP solution and subsequently irradiated with UV light. A comparison with the results previously obtained for non-selective HVP immobilization will be discussed

  19. XPS and AES investigations of the adhesive bonding properties of thin titanium coatings

    International Nuclear Information System (INIS)

    Moers, H.; Mohr, J.; Klewe-Nebenius, H.; Pfennig, G.

    1988-07-01

    The bonding properties of PMMA-microstructures on Ti-coated Cu-substrates after an oxidative treatment in alkaline hydrogenperoxide solution were investigated. In order to clarify the basic mechanism, surface analytical investigations by XPS-, AES-, and depth profile measurements have been performed. It was demonstrated that for optimum bonding a TiO 2 surface layer of ca. 30 nm thickness is necessary. Chemical effects as well as a mechanical bonding with open grain boundary structures (dimensions in the μm-range) could be ruled out as bonding mechanisms. A mechanical interlocking of the polymer with micropores (dimensions in the nm-range) of the oxidic overlayer is adopted as the most probable bonding mechanism. (orig.)

  20. InP/ZnS nanocrystals: coupling NMR and XPS for fine surface and interface description.

    Science.gov (United States)

    Virieux, Héloïse; Le Troedec, Marianne; Cros-Gagneux, Arnaud; Ojo, Wilfried-Solo; Delpech, Fabien; Nayral, Céline; Martinez, Hervé; Chaudret, Bruno

    2012-12-05

    Advanced (1)H, (13)C, and (31)P solution- and solid-state NMR studies combined with XPS were used to probe, at the molecular scale, the composition (of the core, the shell, and the interface) and the surface chemistry of InP/ZnS core/shell quantum dots prepared via a non-coordinating solvent strategy. The interface between the mismatched InP and ZnS phases is composed of an amorphous mixed oxide phase incorporating InPO(x) (with x = 3 and predominantly 4), In(2)O(3), and InO(y)(OH)(3-2y) (y = 0, 1). Thanks to the analysis of the underlying reaction mechanisms, we demonstrate that the oxidation of the upper part of the InP core is the consequence of oxidative conditions brought by decarboxylative coupling reactions (ketonization). These reactions occur during both the core preparation and the coating process, but according to different mechanisms.

  1. Electrochemical capacity fading of polyaniline electrode in supercapacitor: An XPS analysis

    Directory of Open Access Journals (Sweden)

    Jinxing Deng

    2017-04-01

    Full Text Available To understand the electrochemical capacity fading of the polyaniline (PANI electrodes in supercapacitors, for the first time, their chemical structure change during electrochemical cycles was traced with XPS analysis after the HCl doped PANI electrodes were subjected to the cyclic voltammetry test in 1.0 M H2SO4 electrolyte for different cycle numbers. The results showed that the chlorine disappeared in the electrode surface, while the surface element contents of sulfur and oxygen increased with the electrochemical cycles increased. It demonstrated that the hydrolytic degradation of the PANI chains and exchange of dopant occurred during the electrochemical cycling, causing the fading in the mechanical and electrochemical performance of the PANI electrodes. This understanding should lead to better design of the conductive polymer-based energy storage devices.

  2. XPS and TEM study of W-DLC/DLC double-layered film

    International Nuclear Information System (INIS)

    Takeno, Takanori; Komiyama, Takao; Miki, Hiroyuki; Takagi, Toshiyuki; Aoyama, Takashi

    2009-01-01

    A double-layered film of tungsten-containing diamond-like carbon (W-DLC) and DLC, (W-DLC)/DLC, was investigated. A film of 1.6 μm in thickness was deposited onto silicon substrate. The investigate double-layered coating was deposited by using the combination of PECVD and co-sputtering of tungsten metal target. Structure, interface and chemical bonding state of the investigated film were analyzed by Transmission electron microscope (TEM) and X-ray photoelectron spectroscopy (XPS). From the results of the analyses, the structure of double-layered film is that amorphous phase of carbon is continued from DLC to W-DLC and tungsten metal clusters are dispersed in W-DLC layer.

  3. Study on the surface reaction of uranium metal in hydrogen atmosphere with XPS

    International Nuclear Information System (INIS)

    Wang Xiaolin; Fu Yibei; Xie Renshou; Zuo Changming; Zhao Chunpei; Chen Hong

    1998-01-01

    The surface reactions of uranium metal in hydrogen atmosphere at 25 degree C and 200 degree C and effects of temperature and carbon monoxide to the hydriding reaction have been studied by X-ray photoelectron spectroscopy (XPS). The reaction between H 2 and uranium metal at 25 degree C leads to the further oxidation of surface layer of metal due to traces of water vapor. At 200 degree C, it may lead to the hydriding reaction of uranium and the hydriding increases with increasing exposure to H 2 in the initial stages. The U4f 7/2 binding energy of UH 3 has been found to be 378.6 eV. Investigation indicates carbon monoxide inhibits both the hydriding reaction and oxidation on the condition of H 2 -CO atmosphere

  4. Arsenopyrite and pyrite bioleaching: evidence from XPS, XRD and ICP techniques.

    Science.gov (United States)

    Fantauzzi, Marzia; Licheri, Cristina; Atzei, Davide; Loi, Giovanni; Elsener, Bernhard; Rossi, Giovanni; Rossi, Antonella

    2011-10-01

    In this work, a multi-technical bulk and surface analytical approach was used to investigate the bioleaching of a pyrite and arsenopyrite flotation concentrate with a mixed microflora mainly consisting of Acidithiobacillus ferrooxidans. X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and X-ray-induced Auger electron spectroscopy mineral surfaces investigations, along with inductively coupled plasma-atomic emission spectroscopy and carbon, hydrogen, nitrogen and sulphur determination (CHNS) analyses, were carried out prior and after bioleaching. The flotation concentrate was a mixture of pyrite (FeS(2)) and arsenopyrite (FeAsS); after bioleaching, 95% of the initial content of pyrite and 85% of arsenopyrite were dissolved. The chemical state of the main elements (Fe, As and S) at the surface of the bioreactor feed particles and of the residue after bioleaching was investigated by X-ray photoelectron and X-ray excited Auger electron spectroscopy. After bioleaching, no signals of iron, arsenic and sulphur originating from pyrite and arsenopyrite were detected, confirming a strong oxidation and the dissolution of the particles. On the surfaces of the mineral residue particles, elemental sulphur as reaction intermediate of the leaching process and precipitated secondary phases (Fe-OOH and jarosite), together with adsorbed arsenates, was detected. Evidence of microbial cells adhesion at mineral surfaces was also produced: carbon and nitrogen were revealed by CHNS, and nitrogen was also detected on the bioleached surfaces by XPS. This was attributed to the deposition, on the mineral surfaces, of the remnants of a bio-film consisting of an extra-cellular polymer layer that had favoured the bacterial action. © Springer-Verlag 2011

  5. Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

    Science.gov (United States)

    Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

  6. Colloidal diatomite, radionickel, and humic substance interaction: a combined batch, XPS, and EXAFS investigation.

    Science.gov (United States)

    Sheng, Guodong; Shen, Runpu; Dong, Huaping; Li, Yimin

    2013-06-01

    This work determined the influence of humic acid (HA) and fulvic acid (FA) on the interaction mechanism and microstructure of Ni(II) onto diatomite by using batch experiments, X-ray photoelectron spectroscopy (XPS), and extended X-ray absorption fine structure (EXAFS) methods. Macroscopic and spectroscopic experiments have been combined to see the evolution of the interaction mechanism and microstructure of Ni(II) in the presence of HA/FA as compared with that in the absence of HA/FA. The results indicated that the interaction of Ni(II) with diatomite presents the expected solution pH edge at 7.0, which is modified by addition of HA/FA. In the presence of HA/FA, the interaction of Ni(II) with diatomite increased below solution pH 7.0, while Ni(II) interaction decreased above solution pH 7.0. XPS analysis suggested that the enrichment of Ni(II) onto diatomite may be due to the formation of (≡SO)2Ni. EXAFS results showed that binary surface complexes and ternary surface complexes of Ni(II) can be simultaneously formed in the presence of HA/FA, whereas only binary surface complexes of Ni(II) are formed in the absence of HA/FA, which contribute to the enhanced Ni(II) uptake at low pH values. The results observed in this work are important for the evaluation of Ni(II) and related radionuclide physicochemical behavior in the natural soil and water environment.

  7. Difference in surface reactions between titanium and zirconium in Hanks' solution to elucidate mechanism of calcium phosphate formation on titanium using XPS and cathodic polarization

    International Nuclear Information System (INIS)

    Tsutsumi, Y.; Nishimura, D.; Doi, H.; Nomura, N.; Hanawa, T.

    2009-01-01

    Titanium and zirconium were immersed in Hanks' solution with and without calcium and phosphate ions, and the surfaces were characterized with X-ray photoelectron spectroscopy (XPS) to determine the mechanism of calcium phosphate formation on titanium in simulated body fluids and in a living body. In addition, they were cathodically polarized in the above solutions. XPS characterization and cathodic polarization revealed differences in the surface properties in the ability of calcium phosphate formation between titanium and zirconium. The surface oxide film on titanium is not completely oxidized and is relatively reactive; that on zirconium is more passive and protective than that on titanium. Neither calcium nor phosphate stably exists alone on titanium, and calcium phosphate is naturally formed on it; calcium phosphate formed on titanium is stable and protective. On the other hand, calcium is never incorporated on zirconium, while zirconium phosphate, which is easily formed on zirconium, is highly stable and protective. Our study presents new information regarding the surface property of titanium and demonstrates that the characteristics of titanium and zirconium may be applied to various medical devices and new surface modification techniques.

  8. Study of electron beam effects on surfaces using x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectroscopy (SIMS)

    International Nuclear Information System (INIS)

    Gettings, M.; Coad, J.P.

    1976-02-01

    Discrepancies in the surface analyses of oxidised or heavily contaminated materials have been observed between X-ray Photoelectron Spectroscopy (XPS) and techniques using electron beams (primarily Auger Electron Spectroscopy (AES)). These discrepancies can be ascribed to the influence of the primary electron beam and to illustrate the various types of electron effects different materials were analysed using XPS and Secondary Ion Mass Spectroscopy (SIMS) before and after large area electron bombardment. The materials used included chrome and stainless steels, nickel, platinum, glass and brass. (author)

  9. Local mechanical spectroscopy with nanometer-scale lateral resolution

    Science.gov (United States)

    Oulevey, F.; Gremaud, G.; Sémoroz, A.; Kulik, A. J.; Burnham, N. A.; Dupas, E.; Gourdon, D.

    1998-05-01

    A new technique has been developed to probe the viscoelastic and anelastic properties of submicron phases of inhomogeneous materials. The measurement gives information related to the internal friction and to the variations of the dynamic modulus of nanometer-sized volumes. It is then the nanoscale equivalent to mechanical spectroscopy, a well-known macroscopic technique for materials studies, also sometimes called dynamic mechanical (thermal) analysis. The technique is based on a scanning force microscope, using the principle of scanning local-acceleration microscopy (SLAM), and allows the sample temperature to be changed. It is called variable-temperature SLAM, abbreviated T-SLAM. According to a recent proposition to systematize names of scanning probe microscope based methods, this technique should be included in the family of "mechanothermal analysis with scanning microscopy." It is suited for studying defect dynamics in nanomaterials and composites by locating the dissipative mechanisms in submicron phases. The primary and secondary relaxations, as well as the viscoplasticity, were observed in bulk PVC. The wide range of phenomena demonstrate the versatility of the technique. A still unexplained increase of the stiffness with increasing temperature was observed just below the glass transition. All of these observations, although their interpretation in terms of physical events is still tentative, are in agreement with global studies. This technique also permits one to image the variations of the local elasticity or of the local damping at a fixed temperature. This enables the study of, for instance, the homogeneity of phase transitions in multiphased materials, or of the interface morphologies and properties. As an illustration, the homogeneity of the glass transition temperature of PVC in a 50/50 wt % PVC/PB polymer blend has been demonstrated. Due to the small size of the probed volume, T-SLAM gives information on the mechanical properties of the near-surface, which may differ from bulk properties.

  10. Surface refinement and electronic properties of graphene layers grown on copper substrate: An XPS, UPS and EELS study

    Czech Academy of Sciences Publication Activity Database

    Siokou, A.; Ravani, F.; Karakalos, S.; Frank, Otakar; Kalbáč, Martin; Galiotis, C.

    2011-01-01

    Roč. 257, č. 23 (2011), s. 9785-9790 ISSN 0169-4332 R&D Projects: GA MŠk LC510; GA AV ČR IAA400400911 Institutional research plan: CEZ:AV0Z40400503 Keywords : graphene * XPS * EELS Subject RIV: CG - Electrochemistry Impact factor: 2.103, year: 2011

  11. A comparative study of Mg and Pt contacts on semi-insulating GaAs: electrical and XPS characterization

    Czech Academy of Sciences Publication Activity Database

    Dubecký, F.; Kindl, Dobroslav; Hubík, Pavel; Mičušík, M.; Dubecký, M.; Boháček, P.; Vanko, G.; Gombia, E.; Nečas, V.; Mudroň, J.

    2017-01-01

    Roč. 395, Feb (2017), s. 131-135 ISSN 0169-4332 Institutional support: RVO:68378271 Keywords : semi-insulating GaAs * metal -semiconductor contact * interface * work function * electron transport * XPS Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.387, year: 2016

  12. An in situ XPS study of L-cysteine co-adsorbed with water on polycrystalline copper and gold

    Science.gov (United States)

    Jürgensen, Astrid; Raschke, Hannes; Esser, Norbert; Hergenröder, Roland

    2018-03-01

    The interactions of biomolecules with metal surfaces are important because an adsorbed layer of such molecules introduces complex reactive functionality to the substrate. However, studying these interactions is challenging: they usually take place in an aqueous environment, and the structure of the first few monolayers on the surface is of particular interest, as these layers determine most interfacial properties. Ideally, this requires surface sensitive analysis methods that are operated under ambient conditions, for example ambient pressure x-ray photoelectron spectroscopy (AP-XPS). This paper focuses on an AP-XPS study of the interaction of water vapour and l-Cysteine on polycrystalline copper and gold surfaces. Thin films of l-Cysteine were characterized with XPS in UHV and in a water vapour atmosphere (P ≤ 1 mbar): the structure of the adsorbed l-Cysteine layer depended on substrate material and deposition method, and exposure of the surface to water vapour led to the formation of hydrogen bonds between H2O molecules and the COO- and NH2 groups of adsorbed l-Cysteine zwitterions and neutral molecules, respectively. This study also proved that it is possible to investigate monolayers of biomolecules in a gas atmosphere with AP-XPS using a conventional laboratory Al-Kα x-ray source.

  13. Oxygen accumulation on metal surfaces investigated by XPS, AES and LEIS, an issue for sputter depth profiling under UHV conditions

    Energy Technology Data Exchange (ETDEWEB)

    Steinberger, R., E-mail: roland.steinberger@jku.at [Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Celedón, C.E., E-mail: carlos.celedon@usm.cl [Institut für Experimentalphysik, Abteilung für Atom- und Oberflächenphysik, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Departamento de Física, Universidad Técnica Federico Santa María, Valaparaíso, Casilla 110-V (Chile); Bruckner, B., E-mail: barbara.bruckner@jku.at [Institut für Experimentalphysik, Abteilung für Atom- und Oberflächenphysik, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Roth, D., E-mail: dietmar.roth@jku.at [Institut für Experimentalphysik, Abteilung für Atom- und Oberflächenphysik, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Duchoslav, J., E-mail: jiri.duchoslav@jku.at [Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Arndt, M., E-mail: martin.arndt@voestalpine.com [voestalpine Stahl GmbH, voestalpine-Straße 3, 4031 Linz (Austria); Kürnsteiner, P., E-mail: p.kuernsteiner@mpie.de [Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); and others

    2017-07-31

    Highlights: • Investigation on the impact of residual gas prevailing in UHV chambers. • For some metals detrimental oxygen uptake could be observed within shortest time. • Totally different behavior was found: no changes, solely adsorption and oxidation. • The UHV residual gas may severely corrupt results obtained from depth profiling. • A well-considered data acquisition sequence is the key for reliable depth profiles. - Abstract: Depth profiling using surface sensitive analysis methods in combination with sputter ion etching is a common procedure for thorough material investigations, where clean surfaces free of any contamination are essential. Hence, surface analytic studies are mostly performed under ultra-high vacuum (UHV) conditions, but the cleanness of such UHV environments is usually overrated. Consequently, the current study highlights the in principle known impact of the residual gas on metal surfaces (Fe, Mg, Al, Cr and Zn) for various surface analytics methods, like X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and low-energy ion scattering (LEIS). The investigations with modern, state-of-the-art equipment showed different behaviors for the metal surfaces in UHV during acquisition: (i) no impact for Zn, even after long time, (ii) solely adsorption of oxygen for Fe, slight and slow changes for Cr and (iii) adsorption accompanied by oxide formation for Al and Mg. The efficiency of different counter measures was tested and the acquired knowledge was finally used for ZnMgAl coated steel to obtain accurate depth profiles, which exhibited before serious artifacts when data acquisition was performed in an inconsiderate way.

  14. Comparing XPS on bare and capped ZrN films grown by plasma enhanced ALD: Effect of ambient oxidation

    Science.gov (United States)

    Muneshwar, Triratna; Cadien, Ken

    2018-03-01

    In this article we compare x-ray photoelectron spectroscopy (XPS) measurements on bare- and capped- zirconium nitride (ZrN) films to investigate the effect of ambient sample oxidation on the detected bound O in the form of oxide ZrO2 and/or oxynitride ZrOxNy. ZrN films in both bare- and Al2O3/AlN capped- XPS samples were grown by plasma-enhanced atomic layer deposition (PEALD) technique using tetrakis dimethylamino zirconium (TDMAZr) precursor, forming gas (5% H2, rest N2) inductively coupled plasma (ICP), and as received research grade process gases under identical process conditions. Capped samples were prepared by depositing 1 nm thick PEALD AlN on ZrN, followed by additional deposition of 1 nm thick ALD Al2O3, without venting of ALD reactor. On bare ZrN sample at room temperature, spectroscopic ellipsometry (SE) measurements with increasing ambient exposure times (texp) showed a self-limiting surface oxidation with the oxide thickness (dox) approaching 3.7 ± 0.02 nm for texp > 120 min. In XPS data measured prior to sample sputtering (tsput = 0), ZrO2 and ZrOxNy were detected in bare- samples, whereas only ZrN and Al2O3/AlN from capping layer were detected in capped- samples. For bare-ZrN samples, appearance of ZrO2 and ZrOxNy up to sputter depth (dsput) of 15 nm in depth-profile XPS data is in contradiction with measured dox = 3.7 nm, but explained from sputtering induced atomic inter-diffusion within analyzed sample. Appearance of artifacts in the XPS spectra from moderately sputtered (dsput = 0.2 nm and 0.4 nm) capped-ZrN sample, provides an evidence to ion-bombardment induced modifications within analyzed sample.

  15. Cryogenic XPS study of fast-frozen sulfide minerals: Flotation-related adsorption of n-butyl xanthate and beyond

    Energy Technology Data Exchange (ETDEWEB)

    Mikhlin, Yuri, E-mail: yumikh@icct.ru [Institute of Chemistry and Chemical Technology of the Siberian Branch of the Russian Academy of sciences, Akademgorodok, 50/24, Krasnoyarsk 660036 (Russian Federation); Karacharov, Anton; Tomashevich, Yevgeny [Institute of Chemistry and Chemical Technology of the Siberian Branch of the Russian Academy of sciences, Akademgorodok, 50/24, Krasnoyarsk 660036 (Russian Federation); Shchukarev, Andrey [Department of Chemistry, Umeå University, Umeå SE-901 87 (Sweden)

    2016-01-15

    Highlights: • Mineral/aqueous solution interfaces were studied with quasi in situ cryo-XPS. • Dibutyl dixanthogen was the major xanthate adsorption product on pyrite. • Dixanthogen and minor cuprous xanthate were uptaken by chalcopyrite. • Xanthate was chemisorbed at PbS. • Ice-repellent character of hydrophobic particles caused charging effects in XPS. - Abstract: Cryogenic XPS of wet particulate samples separated via centrifugation and fast-frozen allows quasi in situ examination of solid surfaces, adsorbates, and reaction products, largely preventing the loss both of volatiles and hydrated species at mineral/water interfaces. Here, the cryo-XPS has been applied to characterize the surfaces and interfacial layers of natural pyrite (FeS{sub 2}), chalcopyrite (CuFeS{sub 2}), and galena (PbS) in solutions of a common flotation collector, potassium n-butyl xanthate (KBX), in conjunction with zeta-potential measurement. It was found, in particular, that dibutyl dixanthogen was the major adsorbate at pyrite in 0.1 mM KBX and 10 mM KBX solutions; dixanthogen and cuprous xanthate in the next stage were formed on chalcopyrite, and predominant chemisorbed butyl xanthate was present at galena, including in 10 mM KBX solution. The results may suggest that the production of dixanthogens at the interface has been underestimated while the quantities of surface metal xanthates could be over evaluated in previous studies. Pronounced differential charging effects were observed in the XPS experiment for the samples moderately hydrophobized by the xanthate treatment; we proposed that the effect was due to electrically isolated mineral particles with hydrophobic and ice-repellent surfaces, which retained, however, some frozen water islets.

  16. Quantitative chemical state XPS analysis of first row transition metals, oxides and hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Biesinger, M C; Payne, B P; McIntryre, N S [Department of Chemistry, University of Western Ontario, London, Ontario, N6A 5B7 (Canada); Hart, B R; Lau, L Wm [Surface Science Western, Room G1, Western Science Centre, University of Western Ontario, London, Ontario, N6A 5B7 (Canada); Grosvenor, A P [Department of Chemistry, Gunning/Lemieux Chemistry Centre, University of Alberta, Edmonton, Alberta, T6G 2G2 (Canada); Smart, R StC [ACeSSS, Applied Centre for Structural and Synchrotron Studies, University of South Australia, Mawson Lakes, SA 5095 (Australia)], E-mail: biesingr@uwo.ca

    2008-03-15

    Practical quantitative chemical state X-ray photoelectron spectroscopy (XPS) analysis of first row transition metals, oxides and hydroxides is challenging due to the complexity of their M 2p spectra. Complex multiplet splitting, shake-up and plasmon loss structure can play a role in the interpretation of the chemical states present. This paper will show practical curve fitting procedures for the quantitative measurement of different chemical states for metal oxides and hydroxides from a survey of transition metals. It will also discuss some of the limitations and pitfalls present as well as give practical examples of their successful use. These curve-fitting procedures are based on 1) standard spectra from quality reference samples, 2) a survey of appropriate literature databases and/or a compilation of literature references, 3) fitting of multiplet split spectra based on spectra of numerous reference materials and theoretical modelling, 4) spectral subtractions routines, again using reference spectra, and 5) specific literature references where fitting procedures are available.

  17. Quantitative chemical state XPS analysis of first row transition metals, oxides and hydroxides

    International Nuclear Information System (INIS)

    Biesinger, M C; Payne, B P; McIntryre, N S; Hart, B R; Lau, L Wm; Grosvenor, A P; Smart, R StC

    2008-01-01

    Practical quantitative chemical state X-ray photoelectron spectroscopy (XPS) analysis of first row transition metals, oxides and hydroxides is challenging due to the complexity of their M 2p spectra. Complex multiplet splitting, shake-up and plasmon loss structure can play a role in the interpretation of the chemical states present. This paper will show practical curve fitting procedures for the quantitative measurement of different chemical states for metal oxides and hydroxides from a survey of transition metals. It will also discuss some of the limitations and pitfalls present as well as give practical examples of their successful use. These curve-fitting procedures are based on 1) standard spectra from quality reference samples, 2) a survey of appropriate literature databases and/or a compilation of literature references, 3) fitting of multiplet split spectra based on spectra of numerous reference materials and theoretical modelling, 4) spectral subtractions routines, again using reference spectra, and 5) specific literature references where fitting procedures are available

  18. Study of the temperature dependent nitrogen retention in tungsten surfaces by XPS-analysis

    Energy Technology Data Exchange (ETDEWEB)

    Plank, Ulrike [Max-Planck-Institut fuer Plasmaphysik, Boltzmannstr. 2, D-85748 Garching (Germany); Fakultaet fuer Physik der Ludwig-Maximilians-Universitaet Muenchen, Schellingstrasse 4, D-80799 Muenchen (Germany); Meisl, Gerd; Hoeschen, Till [Max-Planck-Institut fuer Plasmaphysik, Boltzmannstr. 2, D-85748 Garching (Germany)

    2016-07-01

    To reduce the power load on the divertor of fusion experiments, nitrogen (N) is puffed into the plasma. As a side effect, nitrogen gets implanted into the tungsten (W) walls of the reactor and forms nitride layers. Their formation and, therefore, the N accumulation in W showed an unexpected temperature dependence in previous experiments. To study the nitrogen retention, we implanted N ions with an energy of 300 eV into W and observed the evolution of the surface composition by X-ray photoelectron spectroscopy (XPS). We find that the N content does not change when the sample is annealed up to 800 K after implantation at lower temperatures. In contrast, the N concentration decreases with increasing implantation temperature. At 800 K implantation temperature, the N saturation level is about 5 times lower compared to 300 K implantation. A possible explanation for this difference is an enhanced diffusion during ion bombardment due to changes in the structure or in the chemical state of the tungsten nitride system. Ongoing tungsten nitride erosion experiments shall help to clarify whether the strong temperature dependence is the result of enhanced diffusion or of phase changes.

  19. XPS and XANES studies of biomimetic composites based on B-type nano-hydroxyapatite

    Science.gov (United States)

    Goloshchapov, D. L.; Gushchin, M. S.; Kashkarov, V. M.; Seredin, P. V.; Ippolitov, Y. A.; Khmelevsky, N. O.; Aksenenko, A. Yu.

    2018-06-01

    The paper presents an investigation of the local atomic structure of nanocrystalline carbonate-substituted hydroxyapatite (CHAP) contained in biomimetic composites - analogues of intact human tooth tissues. Using the XPS technique, the presence of impurity Mg and F atoms and structurally bound carbon in CHAP, at the concentrations typical of apatite enamel and dentine was determined. The XANES method was used to study the changes occurring in P L2,3 spectra of biocomposites with CHAP, depending on the percentage of the amino acid matrix. The appearance of maxima in the spectra of XANES P L2,3 near 135.7 eV for the samples with the composition of amino acid complex/hydroxyapatite - 5/95, 25/75 and the splitting of a broad peak of 146.9 eV in the spectrum of a biocomposite with a composition of 40/60 indicates at the interaction of molecular complex of amino acids with atomic environment of phosphorus. This fact can be used in the fundamental medicine for synthesizing of new biomaterials in dentistry.

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

    International Nuclear Information System (INIS)

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

    1987-01-01

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

  1. X ray photoelectron spectroscopy (XPS) analysis of Photosensitive ZrO2 array

    Science.gov (United States)

    Li, Y.; Zhao, G.; Zhu, R.; Kou, Z.

    2018-03-01

    Based on organic zirconium source as the starting material, by adding chemical modifiers which are made up with photosensitive ZrO2 sol. A uniformed ZrO2 array dot was fabricated with a mean diameter of around 800 nm. By using UV-vis spectra and X-ray photoelectron spectroscopy analysis method, studies the photosensitive ZrO2 gel film of photochemical reaction process and the photosensitive mechanism, to determine the zirconium atom centered chelate structure, reaction formed by metal chelate Zr atom for the center, and to establish the molecular model of the chelate. And studied the ultraviolet light in the process of the variation of the XPS spectra, Zr3d5/2 to 184.9 eV corresponding to the binding energy of the as the combination of state peak gradually reduce; By combining with the status of Zr-O peak gradually increase; The strength of the peak is gradually decline. This suggests that in the process of ultraviolet light photo chemical reaction happened. This study is of great significance to the micro fabrication of ZrO2 array not only to the memory devices but also to the optical devices.

  2. XPS STRUCTURE ANALYSIS OF TiN/TiC BILAYERS PRODUCED BY PULSED VACUUM ARC DISCHARGE

    Directory of Open Access Journals (Sweden)

    ELISABETH RESTREPO PARRA

    2010-01-01

    Full Text Available se crecieron bicapas de TiN/TiC sobre sustratos de acero inoxidable 304 usando un sistema de deposición física de vapor asistida por plasma en forma de arco pulsado a dos diferentes temperaturas del sustrato (50º C y150º C. Para el análisis de la composición química se empleó la técnica de la espectroscopía de fotoelectrones de rayos X (XPS. Se observó el comportamiento de las líneas Ti2p, N1s y C1s. Los análisis de energía de enlace confirmaron la conformación de TiN y TiC. Los picos C1s y Ti2p sufrieron un corrimiento a medida que se incrementó el tiempo de esputtering, revelando contaminación debido a la presencia de hidrocarburos. Además, los perfiles de profundidad de las bicapas de TiN/TiC mostraron que las películas crecidas a una temperatura de 150 ° C tienen una capa de TiN más gruesa que las muestras crecidas a 50º C. El nitrógeno se difundió en la capa de TiC y el carbón en la capa de TiN para ambas temperaturas.

  3. XPS analysis of the effect of fillers on PTFE transfer film development in sliding contacts

    Science.gov (United States)

    Blanchet, T. A.; Kennedy, F. E.; Jayne, D. T.

    1993-01-01

    The development of transfer films atop steel counterfaces in contact with unfilled and bronze-filled PTFE has been studied using X-ray photoelectron spectroscopy. The sliding apparatus was contained within the vacuum of the analytical system, so the effects of the native oxide, hydrocarbon, and adsorbed gaseous surface layers of the steel upon the PTFE transfer behavior could be studied in situ. For both the filled and the unfilled PTFE, cleaner surfaces promoted greater amounts of transfer. Metal fluorides, which formed at the transfer film/counterface interface, were found solely in cases where the native oxide had been removed to expose the metallic surface prior to sliding. These fluorides also were found at clean metal/PTFE interfaces formed in the absence of frictional contact. A fraction of these fluorides resulted from irradiation damage inherent in XPS analysis. PTFE transfer films were found to build up with repeated sliding passes, by a process in which strands of transfer filled in the remaining counterface area. Under these reported test conditions, the transfer process is not expected to continue atop previously deposited transfer films. The bronze-filled composite generated greater amounts of transfer than the unfilled PTFE. The results are discussed relative to the observed increase in wear resistance imparted to PTFE by a broad range of inorganic fillers.

  4. RBS and XPS analyses of the composite calcium phosphate coatings for biomedical applications

    International Nuclear Information System (INIS)

    Ide-Ektessabi, Ari; Yamaguchi, Tetsuro; Tanaka, Yoshikazu

    2005-01-01

    The calcium phosphate coatings on metallic implants are widely used for biomedical applications. The calcium phosphate coatings require mechanical strength, strong adhesion to the metallic implants, chemical stability and low dissolution into the human body fluid for stable functioning in the corrosive environment of the human body. In this study, a novel approach for improving the calcium phosphate coatings is utilized by adding trace metallic element into the coatings. We focused on teeth enamel, which is the hardest calcium phosphate tissue in the human body. Zn concentration increases exponentially from the interior to the surface of the enamel. As the Zn concentration increases, so the local hardness increases. Our previous studies suggest that Zn has influence on the hardness and other properties of enamel, calcium phosphate tissue. Calcium phosphate coatings doped with Zn was fabricated and characterized. The atomic composition and chemical state were investigated by using Rutherford backscattering spectroscopy (RBS) and X-ray photoelectron spectrometer (XPS), respectively. Scratch test was also carried out for measuring the adhesion of the coatings

  5. XPS and XAES measurements on trapped rare gases in transition metals

    International Nuclear Information System (INIS)

    Baba, Y.; Yamamoto, H.; Sasaki, T.A.

    1992-01-01

    Electronic structures of rare gases implanted in various transition metals have been investigated by means of an X-ray photoelectron spectroscopy (XPS) and X-ray-induced Auger electron spectroscopy (XAES). The Auger-parameter method is applied to the evaluation of electronic relaxation energy of rare gas atoms due to the surrounding metal potential. The extra-atomic relaxation energy of four kinds of rare gases (Ne, Ar, Kr, Xe) in the same metal matrix (Ti) increases with the atomic mass of the rare gases. On the other hand, the extra-atomic relaxation energy of the same rare gas (Xe) in different metal matrices ranges from 3.0 eV (in Mo). These values increase with the number of d-electrons in the metals. This tendency and the absolute values of the relaxation energies are in good agreement with those calculated for 3d transition metals referenced to their gas-phase values. Based on these results, it is concluded that the energetically implanted rare gases are trapped at the substitution site in the metal lattice as an isolated atom, and the trapped atoms feel the surrounding metal potential. It is also made clear that the potential affecting the implanted atom is d-like, and the relaxation energy of the implanted rare gas during the photoemission process is almost equal to those of the metal itself. (orig.)

  6. Influence of the lithium salt nature over the surface film formation on a graphite electrode in Li-ion batteries: An XPS study

    International Nuclear Information System (INIS)

    Leroy, S.; Martinez, H.; Dedryvere, R.; Lemordant, D.; Gonbeau, D.

    2007-01-01

    The formation of a passivation film (solid electrolyte interphase, SEI) at the surface of the negative electrode of full LiCoO 2 /graphite lithium-ion cells using different salts (LiBF 4 , LiPF 6 , LiTFSI, LiBETI) in carbonate solvents as electrolyte was investigated by X-ray photoelectron spectroscopy (XPS). The analyzes were carried out at different potential stages of the first cycle, showing the potential-dependent character of the surface film species formation and the specificity of each salt. At 3.8 V, for all salts, we have mainly identified carbonated species. Beyond this potential, the specific behavior of LiPF 6 was identified with a high LiF deposit, whereas for other salts, the formation process of the SEI appears controlled by the solvent decomposition of the electrolyte

  7. [XPS analysis of beads formed by fuse breaking of electric copper wire].

    Science.gov (United States)

    Wu, Ying; Meng, Qing-Shan; Wang, Xin-Ming; Gao, Wei; Di, Man

    2010-05-01

    The in-depth composition of beads formed by fuse breaking of the electric copper wire in different circumstances was studied by XPS with Ar+ ion sputtering. In addition, the measured Auger spectra and the calculated Auger parameters were compared for differentiation of the substances of Cu and Cu2O. Corresponding to the sputtering depth, the molten product on a bead induced directly by fuse breaking of the copper wire without cover may be distinguished as three portions: surface layer with a drastic decrease in carbon content; intermediate layer with a gentle change in oxygen content and gradually diminished carbon peak, and consisting of Cu2O; transition layer without Cu2O and with a rapid decrease in oxygen content. While the molten product on a bead formed by fuse breaking of the copper wire after its insulating cover had been burned out may be distinguished as two portions: surface layer with carbon content decreasing quickly; subsurface layer without Cu2O and with carbon and oxygen content decreasing gradually. Thus, it can be seen that there was an obvious interface between the layered surface product and the substrate for the first type of bead, while as to the second type of bead there was no interface. As a result, the presence of Cu2O and the quantitative results can be used to identify the molten product on a bead induced directly by fuse breaking of the copper wire without cover and the molten product on a bead formed by fuse breaking of the cupper wire after its insulating cover had been burned out, as a complementary technique for the judgments of fire cause.

  8. Characterization study of native oxides on GaAs(100) surface by XPS

    Science.gov (United States)

    Feng, Liu; Zhang, Lian-dong; Liu, Hui; Gao, Xiang; Miao, Zhuang; Cheng, Hong-chang; Wang, Long; Niu, Sen

    2013-08-01

    In order to know more about the surface state of GaAs(100) epitaxial wafer during a storage period of two years, the XPS analysis was carried out four times on the surface, respectively polished by chemical etching, stored in desiccator for half a year, one year and two years. The results indicated that even after cleaned by proper etchant solutions, the fresh surface was slightly oxidized with Ga2O3, As2O3 and organic contaminant. The epi-wafer was always exposed to air during the storage period, so more and more oxides turned out. The mixed oxide layer comprised of C-OR, COOR, Ga2O3, As2O3 and As2O5 appeared after only half a year. In the ageing process of two years, the oxide types of gallium or arsenic did not change with stable content of Ga2O3 and remarkably fluctuating relative contents of As2O3 and As2O5. Based on the intensity ratio of Ga 3d-Ga2O3 to Ga 3d-GaAs, the thickness of oxide layer was estimated. The oxide layer generated after chemical polishing was very thin, just only 0.435nm thick, and then it grew rapidly, approximately 1.822nm after one year while almost no change any more subsequently. It was indicated that after the epi-wafer was stored for one year, because of volatile As2O3 or As2O5, there remained a large amount of Ga2O3 in oxide layer, which prevented the reactions between bulk material and oxide layer with oxygen. So native oxide layer plays a role as passive film to protect epi-wafer against the environment during a long storage period.

  9. Raman and XPS characterization of vanadium oxide thin films with temperature

    Energy Technology Data Exchange (ETDEWEB)

    Ureña-Begara, Ferran, E-mail: ferran.urena@uclouvain.be [Université catholique de Louvain, Institute of Information and Communication Technologies, Electronics and Applied Mathematics (ICTEAM), Louvain-la-Neuve (Belgium); Crunteanu, Aurelian [XLIM Research Institute, UMR 7252, CNRS/Université de Limoges, Limoges (France); Raskin, Jean-Pierre [Université catholique de Louvain, Institute of Information and Communication Technologies, Electronics and Applied Mathematics (ICTEAM), Louvain-la-Neuve (Belgium)

    2017-05-01

    Highlights: • Comprehensive study of the oxidation of VO{sub 2} thin films from R.T. up to 550 °C. • Phase changes and mixed-valence vanadium oxides formed during the oxidation process. • Reported Raman and XPS signatures for each vanadium oxide. • Monitoring of the current and resistance evolution at the surface of the films. • Oxidation model describing the evolution of the vanadium oxides and phase changes. - Abstract: The oxidation mechanisms and the numerous phase transitions undergone by VO{sub 2} thin films deposited on SiO{sub 2}/Si and Al{sub 2}O{sub 3} substrates when heated from room temperature (R.T.) up to 550 °C in air are investigated by Raman and X-ray photoelectron spectroscopy. The results show that the films undergo several intermediate phase transitions between the initial VO{sub 2} monoclinic phase at R.T. and the final V{sub 2}O{sub 5} phase at 550 °C. The information about these intermediate phase transitions is scarce and their identification is important since they are often found during the synthesis of vanadium dioxide films. Significant changes in the film conductivity have also been observed to occur associated to the phase transitions. In this work, current and resistance measurements performed on the surface of the films are implemented in parallel with the Raman measurements to correlate the different phases with the conductivity of the films. A model to explain the oxidation mechanisms and phenomena occurring during the oxidation of the films is proposed. Peak frequencies, full-width half-maxima, binding energies and oxidation states from the Raman and X-ray photoelectron spectroscopy experiments are reported and analyzed for all the phases encountered in VO{sub 2} films prepared on SiO{sub 2}/Si and Al{sub 2}O{sub 3} substrates.

  10. XPS and SIMS characterisation of TiOxNy solar absorber films

    International Nuclear Information System (INIS)

    Metson, J.B.; Prince, K.E.; Bittar, A.; Tornquist, J.

    1999-01-01

    Full text: TiO x N y thin films have useful properties as selective solar absorbers when used in tandem with a collector substrate. Such films are transparent across a reasonable window of the solar spectrum, but have low thermal emissivity. They are however limited by their thermal stability under the typical operating conditions they experience. In this study, TiO x N y films have been deposited on Si and Cu substrates using ion beam assisted deposition. The films are amorphous and x and y were controlled by altering the O 2 /N 2 ratio in the gas source. After annealing at temperatures of 200 - 400 deg C, films have been depth profiled using Secondary Ion Mass Spectrometry. Profiles reveal the degradation of the film by migration of the substrate atoms through the films, to the sample surface. In general, films with x 1 show improved stability, ultimately at the expense of a reduced transmission window. Thermal stability is also improved by the use of diffusion barriers either at the substrate film interface or at the surface of the film. However contrary to previous suggestions, the degradation mechanism involves the formation not of an oxide at the film surface but a phase which is nitrogen rich. The nature of this phase, formed by diffusion of the substrate atoms, has been investigated by X-ray photoelectron spectroscopy (XPS). These investigations reveal very complex behaviour in the early stages of film failure, with an almost intact TiO x N y layer surviving, but being progressively buried by the growth of the reaction layer at the film surface. Copyright (1999) Australian X-ray Analytical Association Inc

  11. XPS investigation of monatomic and cluster argon ion sputtering of tantalum pentoxide

    Energy Technology Data Exchange (ETDEWEB)

    Simpson, Robin, E-mail: r.simpson@surrey.ac.uk [The Surface Analysis Laboratory, Department of Mechanical Engineering Sciences, University of Surrey (United Kingdom); Thermo Scientific, East Grinstead (United Kingdom); White, Richard G. [Thermo Scientific, East Grinstead (United Kingdom); Watts, John F.; Baker, Mark A. [The Surface Analysis Laboratory, Department of Mechanical Engineering Sciences, University of Surrey (United Kingdom)

    2017-05-31

    Highlights: • Ion beam induced oxide reduction from monatomic and gas cluster ion beam exposure are compared. • Lower relative level of preferential sputtering is shown in gas cluster ion beam depth profiling. • A lack of “steady state” is observed in gas cluster ion beam depth profiles of tantalum pentoxide. • Possible mechanisms behind the observed results, including temperature effects are proposed. - Abstract: In recent years, gas cluster ion beams (GCIB) have become the cutting edge of ion beam technology to sputter etch organic materials in surface analysis. However, little is currently known on the ability of argon cluster ions (Ar{sub n}{sup +}) to etch metal oxides and other technologically important inorganic compounds and no depth profiles have previously been reported. In this work, XPS depth profiles through a certified (European standard BCR-261T) 30 nm thick Ta{sub 2}O{sub 5} layer grown on Ta foil using monatomic Ar{sup +} and Ar{sub 1000}{sup +} cluster ions have been performed at different incident energies. The preferential sputtering of oxygen induced using 6 keV Ar{sub 1000}{sup +} ions is lower relative to 3 keV and 500 eV Ar{sup +} ions. Ar{sup +} ions exhibit a steady state O/Ta ratio through the bulk oxide but Ar{sub 1000}{sup +} ions show a gradual decrease in the O/Ta ratio as a function of depth. The depth resolution and etch rate is substantially better for the monatomic beam compared to the cluster beam. Higher O concentrations are observed when the underlying Ta bulk metal is sputtered for the Ar{sub 1000}{sup +} profiles compared to the Ar{sup +} profiles.

  12. The determination of acid-base properties of polymer surfaces by XPS: Present status and future prospects

    International Nuclear Information System (INIS)

    Chehimi, M.M.; Delamar, M.; Shahidzadeh-Ahmadi, N.; Arefi-Khonsari, F.; Amouroux, J.; Watts, J.F.

    1996-01-01

    The use of the molecular probe technique in conjunction with X-ray photoelectron spectroscopy (XPS) for the assessment of acid-base properties of polymer surfaces is reviewed. The method is based on the determination of the concentration and chemical shifts of Lewis acids (bases) sorbed in polymers of basic (acidic) character. In the case of chloroform (Lewis acid) sorbed in polymers of Lewis basic character, C12p binding energy is linearly correlated with ΔH AB , the heat of acid-base complex formation chloroform-polymer. This relationship has been used to determine the acid-base properties of poly(phenylene oxide), a homopolymer, and ammonia plasma-treated polypropylene. This work shows that XPS can now indeed be used to quantitatively assess the acid-base properties of modified polymer surfaces and perhaps be extended to map acid-base properties of polymer surfaces at the micron or submicron scale. copyright 1996 American Institute of Physics

  13. Growth of TiC films by Pulsed Laser Evaporation (PLE) and characterization by XPS and AES

    International Nuclear Information System (INIS)

    Rist, O.; Murray, P.T.

    1991-01-01

    Thin films of TiC with a thickness of some 100 nm have been grown on Si(100) substrates by Pulsed Laser Evaporation (PLE). Advantages of PLE in comparison with more conventional growth methods e.g. PVD or CVD are reported. The feasibility of growing stoichiometric thin films of TiC by PLE was investigated. These films produced have been analysed in situ by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). XPS results and Auger sputter depht profiles indicate that the films grown between RT and 500degC are stoichiometric TiC. Film/substrate interdiffusion is observed at 600degC substrate temperature and higher. (orig.)

  14. XPS study of U, UNi5, UCu5 and UNisub(0.5)Cusub(4.5)

    International Nuclear Information System (INIS)

    Grohs, H.; Hoechst, H.; Steiner, P.; Huefner, S.; Buschow, K.H.J.

    1980-01-01

    Core and valence band spectra of U metal and the intermetallic compounds UNi 5 , UCu 5 and UNisub(0.5)Cusub(4.5) have been measured by X-ray excited photoelectron spectroscopy (XPS). The data indicate that in UNi 5 the configuration is 5f 3 , and in UCu 5 and UNisub(0.5)Cusub(4.5) a mixed valence configuration with fewer 5f electrons than in UNi 5 is present. (author)

  15. XPS and SIMS study of aluminium native oxide modifications induced by Q-switched Nd :YAG laser treatment

    CSIR Research Space (South Africa)

    Barnier, V

    2006-04-01

    Full Text Available with fluences between 0.7 and 1.7 J/cm2, X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectroscopy (SIMS) revealed thermal oxidation with an increase of the oxide-layer thickness for 0.7–1.3 J/cm2. Above a threshold at about 1.3 J/cm2 the oxide...

  16. Peak position differences observed during XPS sputter depth profiling of the SEI on lithiated and delithiated carbon-based anode material for Li-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Oswald, S., E-mail: s.oswald@ifw-dresden.de; Hoffmann, M.; Zier, M.

    2017-04-15

    Highlights: • In XPS measurements at graphite anodes for Li-ion batteries specific binding energy variations are observed for the SEI species. • The binding energy variations depend on the charging state of the graphite and not on surface charging effects. • Obviously the presence of elemental Li leads to a potential surface gradient in contact with surface layers. • The energy position of implanted Ar can be used as characteristic feature during sputter depth profiling experiments. - Abstract: The ability of delivering chemical information from peak shift phenomena has ever since made X-ray photoelectron spectroscopy (XPS) an ideal tool for material characterization in Li-ion batteries (LIB). Upon investigation, charging is inevitable as most of the chemical species involved are non-conducting. Thus, the binding energy (BE) scale must be corrected to allow an accurate interpretation of the results. This is usually done using the peak position of the ubiquitous surface carbon contamination detectable for all Li-ion battery relevant materials. We herein report on the occurrence of peak shift phenomena that can be observed when investigating surface layers on graphite anodes using sputter depth-profiling. These shifts, however, are not related to classical static electric charging, but are depending on the state of charge (lithiation) of the anode material. The observations presented are in agreement with previous findings on other Li-containing materials and are obviously caused by the presence of Li in its elemental state. As aging and failure mechanisms in LIBs are closely linked to electrolyte reaction products on electrode surfaces it is of high importance to draw the correct conclusions on their chemical origin from XP spectra. In order to avoid misinterpretation of the BE positions, implanted Ar can be used for identification of relevant peak positions and species involved in the phenomena observed.

  17. Positive XPS binding energy shift of supported Cu{sub N}-clusters governed by initial state effects

    Energy Technology Data Exchange (ETDEWEB)

    Peters, S.; Peredkov, S. [Technische Universität Berlin, IOAP, Strasse des 17. Juni 135, 10623 Berlin (Germany); Al-Hada, M. [Department of Physics, College of Education and Linguistics, University of Amran (Yemen); Neeb, M., E-mail: matthias.neeb@helmholtz-berlin.de [Helmholtz-Zentrum Berlin, Wilhelm-Conrad-Röntgen-Campus Adlershof, Elektronenspeicherring BESSY II, Albert-Einstein-Straße 15, 12489 Berlin (Germany); Eberhardt, W. [Technische Universität Berlin, IOAP, Strasse des 17. Juni 135, 10623 Berlin (Germany); DESY, Center for Free Electron Laser Science (CFEL), Notkestr. 85, 22607 Hamburg (Germany)

    2014-01-01

    Highlights: • Size dependent initial and final state effects of mass-selected deposited clusters. • Initial state effect dominates positive XPS shift in supported Cu-clusters. • Size dependent Coulomb correlation shift in the Auger final state of Cu cluster. • Size-dependent Auger parameter analysis. • Positive XPS shift differs from negative surface core level shift in crystalline copper. - Abstract: An initial state effect is established as origin for the positive 2p core electron binding energy shift found for Cu{sub N}-clusters supported by a thin silica layer of a p-doped Si(1 0 0) wafer. Using the concept of the Auger parameter and taking into account the usually neglected Coulomb correlation shift in the Auger final state (M{sub 4,5}M{sub 4,5}) it is shown that the initial state shift is comparable to the measured XPS shift while the final state relaxation shift contributes only marginally to the binding energy shift. The cluster results differ from the negative surface core-level shift of crystalline copper which has been explained in terms of a final state relaxation effect.

  18. Temperature dependent structural, luminescent and XPS studies of CdO:Ga thin films deposited by spray pyrolysis

    International Nuclear Information System (INIS)

    Moholkar, A.V.; Agawane, G.L.; Sim, Kyu-Ung; Kwon, Ye-bin; Choi, Doo Sun; Rajpure, K.Y.; Kim, J.H.

    2010-01-01

    Research highlights: → The CdO:Ga thin films seems an alternative to traditional TCO materials used in photovoltaic applications. This work deals the effect of deposition temperature on sprayed CdO:Ga films with respect to the structural, luminescent and XPS studies. → The crystalline quality of the GCO films improves with deposition temperature. → The oxygen vacancies are responsible for n-type conductivity and green emission. → The minimum resistivity, highest carrier concentration and mobility are 1.9 x 10 -4 Ω cm, 11.7 x 10 21 cm -3 and 27.64 cm 2 V -1 s -1 , respectively. - Abstract: The structural, compositional, photoluminescent and XPS properties of CdO:Ga thin films deposited at temperatures ranging from 275 to 350 o C, using spray pyrolysis are reported. X-ray diffraction characterization of as-deposited GCO thin films reveals that films are of cubic structure with a (2 0 0) preferred orientation. The crystalline quality of the GCO films improves and the grain size increases with deposition temperature. The EDS analyses confirm oxygen deficiency present in the film and are responsible for n-type conductivity. The photoluminescence spectra demonstrated that the green emission peaks of CdO thin films are centered at 482 nm. The relative intensity of these peaks is strongly dependent on the deposition temperature. Oxygen vacancies are dominant luminescent centers for green emission in CdO thin films. The XPS measurement shows the presence of Cd, Ga, O and C elements and confirms that CdO:Ga films are cadmium-rich.

  19. An IR and XPS spectroscopy assessment of the physico-chemical surface properties of alumina–YAG nanopowders

    Energy Technology Data Exchange (ETDEWEB)

    Spina, Giulia; Bonelli, Barbara, E-mail: barbara.bonelli@polito.it; Palmero, Paola, E-mail: paola.palmero@polito.it; Montanaro, Laura

    2013-12-16

    Well-dispersed nano-crystalline transition alumina suspensions were mixed with yttrium chloride aqueous solutions, with the aim of producing by spray-drying Al{sub 2}O{sub 3}–Y{sub 3}Al{sub 5}O{sub 12} (YAG) composite powders of increasing YAG vol.%. Two samples were prepared, with different Y content, corresponding to 5 and 20 YAG vol.%, respectively. Both samples were then treated at either 600 or 1150 °C. The obtained powders were characterized by X-Ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Fourier Transform Infra Red (FT-IR) spectroscopy and compared to three reference samples: commercial nano-crystalline transition alumina, YAG and Y{sub 2}O{sub 3}. YAG powders were obtained by co-precipitation route whereas Y{sub 2}O{sub 3} powders were yielded by spray-drying of a yttrium chloride aqueous solution. Modification of physico-chemical properties of the surface of alumina nanoparticles were assessed by combining XPS and FT-IR spectroscopies. On the basis of the results obtained, a possible model is proposed for the structure of the obtained composites, in which Y basically reacts with more acidic hydroxyls of alumina, by forming Y-rich surface grains, the extension of which depends on the thermal treatment. - Highlights: • Al{sub 2}O{sub 3}–Y{sub 3}Al{sub 5}O{sub 12} (YAG) composite nanopowders were prepared by spray drying. • Combined XPS and IR spectroscopy: effective tools to study surface modifications. • Y reacts with more acidic hydroxyls at alumina surface. • Y-rich surface grains form: their extension depends on the thermal treatment.

  20. Solar Ion Processing of Major Element Surface Compositions of Mature Mare Soils: Insights from Combined XPS and Analytical TEM Observations

    Science.gov (United States)

    Christoffersen, R.; Dukes, C.; Keller, L. P.; Baragiola, R.

    2012-01-01

    Solar wind ions are capable of altering the sur-face chemistry of the lunar regolith by a number of mechanisms including preferential sputtering, radiation-enhanced diffusion and sputter erosion of space weathered surfaces containing pre-existing compositional profiles. We have previously reported in-situ ion irradiation experiments supported by X-ray photoelectron spectroscopy (XPS) and analytical TEM that show how solar ions potentially drive Fe and Ti reduction at the monolayer scale as well as the 10-100 nm depth scale in lunar soils [1]. Here we report experimental data on the effect of ion irradiation on the major element surface composition in a mature mare soil.

  1. XPS study on the electronic structure of hydrided Ti-V, Ti-Nb and Ti-Mo alloys

    International Nuclear Information System (INIS)

    Tanaka, Kazuhide; Aoki, Hiromasa

    1989-01-01

    Effects of hydrogenation on the core and valence electronic structures of β(bcc)-stabilized Ti-25at%V, Ti-50at%Nb and Ti-20at%Mo alloys are studied with XPS technique using monochromatized Al K α radiation. Small but uniform binding-energy shifts are observed upon hydrogenation for all the core spectra measured. Their valence-band spectra are significantly distorted, providing an evidence of the formation of metal-hydrogen bonding bands in these Ti alloys. Interrelations between the core binding-energy shifts and the valence-band distortion are discussed. (orig.)

  2. Characterization of uranium bioaccumulation on a fungal isolate Geotrichum sp. dwc-1 as investigated by FTIR, TEM and XPS

    International Nuclear Information System (INIS)

    Changsong Zhao; Congcong Ding; Jiali Liao; Jijun Yang; Yuanyou Yang; Jun Tang; Ning Liu; Qun Sun

    2016-01-01

    In this paper, TEM-EDX, FTIR, XPS, PIXE, and EPBS were employed to identify the uranium biosorption behavior and the potential mechanism on cells of Geotrichum sp. dwc-1, isolated from soils. These results displayed that the biosorption behavior was greatly dependent on pH and uranium was absorbed by bounding to amino, phosphate as well as carboxyl functional groups. Uranium biosorption behavior on Geotrichum sp. dwc-1 involves bioaccumulation, electrostatic interaction and ion exchange process. This work throws further light on potential fungal roles these mechanisms for elemental recovery and bioremediation. (author)

  3. Tracking the conversion of nitrogen during pyrolysis of antibiotic mycelial fermentation residues using XPS and TG-FTIR-MS technology

    International Nuclear Information System (INIS)

    Zhu, Xiangdong; Yang, Shijun; Wang, Liang; Liu, Yuchen; Qian, Feng; Yao, Wenqing; Zhang, Shicheng; Chen, Jianmin

    2016-01-01

    Antibiotic mycelial fermentation residues (AMFRs), which are emerging solid pollutants, have been recognized as hazardous waste in China since 2008. Nitrogen (N), which is an environmental sensitivity element, is largely retained in AMFR samples derived from fermentation substrates. Pyrolysis is a promising technology for the treatment of solid waste. However, the outcomes of N element during the pyrolysis of AMFRs are still unknown. In this study, the conversion of N element during the pyrolysis of AMFRs was tracked using XPS (X-ray photoelectron spectroscopy) and online TG-FTIR-MS (Thermogravimetry-Fourier transform infrared-Mass spectrometry) technology. In the AMFR sample, organic amine-N, pyrrolic-N, protein-N, pyridinic-N, was the main N-containing species. XPS results indicated that pyrrolic-N and pyridinic-N were retained in the AMFR-derived pyrolysis char. More stable species, such as N-oxide and quaternary-N, were also produced in the char. TG-FTIR-MS results indicated that NH_3 and HCN were the main gaseous species, and their contents were closely related to the contents of amine-N and protein-N, and pyrrolic-N and pyridinic-N of AMFRs, respectively. Increases in heating rate enhanced the amounts of NH_3 and HCN, but had less of an effect on the degradation degree of AMFRs. N-containing organic compounds, including amine-N, nitrile-N and heterocyclic-N, were discerned from the AMFR pyrolysis process. Their release range was extended with increasing of heating rate and carbon content of AMFR sample. This work will help to take appropriate measure to reduce secondary pollution from the treatment of AMFRs. - Highlights: • Hazardous AMFR material was treated by slow pyrolysis reaction. • TG-FTIR-MS were used to study the N conversion for pyrolysis gas and bio-oil. • NH_3 and HCN were observed as the main N-containing gas species. • XPS were used to study the N conversion for pyrolysis char. • Stable species, such as N-oxide and quaternary-N, were

  4. Atomic and Nuclear Analytical Methods XRF, Mössbauer, XPS, NAA and Ion-Beam Spectroscopic Techniques

    CERN Document Server

    Verma, H R

    2007-01-01

    This book is a blend of analytical methods based on the phenomenon of atomic and nuclear physics. It comprises comprehensive presentations about X-ray Fluorescence (XRF), Mössbauer Spectroscopy (MS), X-ray Photoelectron Spectroscopy (XPS), Neutron- Activation Analysis (NAA), Particle Induced X-ray Emission Analysis (PIXE), Rutherford Backscattering Analysis (RBS), Elastic Recoil Detection (ERD), Nuclear Reaction Analysis (NRA), Particle Induced Gamma-ray Emission Analysis (PIGE), and Accelerator Mass Spectrometry (AMS). These techniques are commonly applied in the fields of medicine, biology, environmental studies, archaeology or geology et al. and pursued in major international research laboratories.

  5. In-situ XPS analysis of oxidized and reduced plasma deposited ruthenium-based thin catalytic films

    Science.gov (United States)

    Balcerzak, Jacek; Redzynia, Wiktor; Tyczkowski, Jacek

    2017-12-01

    A novel in-situ study of the surface molecular structure of catalytically active ruthenium-based films subjected to the oxidation (in oxygen) and reduction (in hydrogen) was performed in a Cat-Cell reactor combined with a XPS spectrometer. The films were produced by the plasma deposition method (PEMOCVD). It was found that the films contained ruthenium at different oxidation states: metallic (Ru0), RuO2 (Ru+4), and other RuOx (Ru+x), of which content could be changed by the oxidation or reduction, depending on the process temperature. These results allow to predict the behavior of the Ru-based catalysts in different redox environments.

  6. XPS Analysis of Ni and Oxygen in Single-Sintered SrTiO3 Multifunction Ceramic

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    XPS analyses have been performed to investigate the chemical conditions of Ni and oxygen on grain surfaces in single-sintered SrTiO3 capacitor-varistor ceramic doped with Nb2O5 and NiO. It is ascertained that Ni is in form of Ni2+ ions, which substitute for Ti4+ ions on grain surfaces during the oxidizing annealing. Moreover, it is confirmed that three kinds of chemically adsorbed oxygen such as O2-, O- and O~ are formed on grain surfaces. It is proposed that these behaviors contribute greatly to the generation of multiple types of grain boundary acceptor states in the ceramic.

  7. XPS study on the surface reaction of uranium metal in H2 and H2-CO atmospheres

    International Nuclear Information System (INIS)

    Wang Xiaolin; Fu Yibei; Xie Renshou

    1996-04-01

    The surface reactions of uranium metal in H 2 and H 2 -CO atmospheres and the effects of temperature and CO on the hydriding reaction have been studied by X-ray photoelectron spectroscopy (XPS). The reaction between commercial H 2 and uranium metal at 25 degree C leads mainly to the further oxidation of surface layer of metal due to traces of water vapour. At 200 degree C, it may lead to the hydriding reaction of uranium and the hydriding increases with increasing the exposure of H 2 . Investigation indicates CO inhibits both the hydriding reaction and oxidation on the condition of H 2 -CO atmospheres. (13 refs., 10 figs.)

  8. XPS and GDOES Characterization of Porous Coating Enriched with Copper and Calcium Obtained on Tantalum via Plasma Electrolytic Oxidation

    Directory of Open Access Journals (Sweden)

    Krzysztof Rokosz

    2016-01-01

    Full Text Available XPS and GDOES characterizations of porous coatings on tantalum after Plasma Electrolytic Oxidation (PEO at 450 V for 3 minutes in electrolyte containing concentrated (85% phosphoric acid with calcium nitrate and copper (II nitrate are described. Based on the obtained data, it may be concluded that the PEO coating consists of tantalum (Ta5+, calcium (Ca2+, copper (Cu2+  and Cu+, and phosphates (PO43-. It has to be pointed out that copper and calcium are distributed throughout the volume. The authors also propose a new model of PEO, based on the derivative of GDOES signals with sputtering time.

  9. XPS-and-DFT analyses of the Pb 4f — Zn 3s and Pb 5d — O 2s overlapped ambiguity contributions to the final electronic structure of bulk and thin-film Pb-modulated zincite

    Energy Technology Data Exchange (ETDEWEB)

    Zatsepin, D.A. [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, 620990 Yekaterinburg (Russian Federation); Institute of Physics and Technology, Ural Federal University, 620002 Yekaterinburg (Russian Federation); Boukhvalov, D.W., E-mail: danil@hanyang.ac.kr [Department of Chemistry, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Theoretical Physics and Applied Mathematics Department, Ural Federal University,Mira Street 19, 620002 Yekaterinburg (Russian Federation); Gavrilov, N.V. [Institute of Electrophysics, Russian Academy of Sciences, Ural Branch, 620990 Yekaterinburg (Russian Federation); Kurmaev, E.Z. [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, 620990 Yekaterinburg (Russian Federation); Institute of Physics and Technology, Ural Federal University, 620002 Yekaterinburg (Russian Federation); Zatsepin, A.F. [Institute of Physics and Technology, Ural Federal University, 620002 Yekaterinburg (Russian Federation); Cui, L. [Shenzhen Graduate School, Harbin Institute of Technology, Shenzhen 518055 (China); Shur, V. Ya.; Esin, A.A. [Institute of Natural Sciences, Ural Federal University, 51 Lenin Ave, 620000 Yekaterinburg (Russian Federation)

    2017-05-31

    Highlights: • Two modes of ZnO:Pb in the bulk and surface morphologies were established: the high- and low-interaction. • It was shown the ambiguity contribution of Pb 4f − Zn 3s and Pb 5d − O 2s states into final electronic structure. • The main type of defects is PbO-like with some PbO{sub 2}-like contributions. • An applied wurzite-like structural model well agrees with experimental data obtained for zincite. - Abstract: The electronic structures of zincite Pb-modulated bulk and thin-films were studied via X-ray photoelectron spectroscopy (XPS) and density functional theory (DFT) techniques. Both XPS data and DFT-calculations allowed the derivation of two different Pb-embedding scenarios into the ZnO-hosts. These included the high-interaction mode of Pb-impurity with initial zinc-oxygen host-lattice for the bulk morphology, accompanied with low Pb-metal losses; and the low-interaction mode for thin-films, where there was intake of Pb-impurities into the hollows of the surface. Despite dissimilar mechanisms of Pb-impurity accumulation and distribution in the bulk and thin-films zincite host-matrices, the strong Pb 4f — Zn 3s and Pb 5d — O 2s overlapped ambiguity contribution to the appropriate core-level structure and valence bands was established by XPS analysis and reproduced with the help of DFT-calculations. It was shown that the microscopic structure of the embedded lead-impurity played a crucial role in the Pb ion-beam stimulated synthesis of secondary lead-oxygen phases via large-area defect fabrication, and the difference among zincite and wurzite polymorphs played almost no role in this case.

  10. Characterization of Sr2+ uptake on natural minerals of kaolinite and magnesite using XRPD, SEM/EDS, XPS, and DRIFT

    International Nuclear Information System (INIS)

    Shahwan, T.; Erten, H.N.

    2005-01-01

    The sorption behavior of Sr 2+ ions on natural minerals rich in kaolinite and magnesite was studied using SEM/EDS, XPS, XRPD, AAS/AES and DRIFT techniques. Quantitative analysis of the XPS data shows that magnesite is more effective in Sr 2+ uptake than kaolinite. DRIFT spectra and XRPD patterns indicate that the structures of both minerals were not affected upon Sr 2+ sorption. Intercalation of DMSO in kaolinite lamellae aiming at increasing the interlayer space did not significantly enhance the sorption capacity of the clay towards Sr 2+ probably due to the lack of a negative charge on the accessible sites. EDS mapping indicated that while the sorbed Sr is equally distributed on surface of natural kaolinite, it was associated - to a larger extent - with the regions richer in Mg in the case of natural magnesite. Comparing the uptake mechanisms of natural magnesite with that of pure MgCO 3 , it was seen that while natural magnesite sorbed Sr 2+ mainly through an ion exchange type mechanism, the formation of SrCO 3 coprecipitate was detected on the surface of the MgCO 3 at higher loadings. (orig.)

  11. Initial surface film on magnesium metal: A characterization by X-ray photoelectron spectroscopy (XPS) and photocurrent spectroscopy (PCS)

    International Nuclear Information System (INIS)

    Santamaria, M.; Di Quarto, F.; Zanna, S.; Marcus, P.

    2007-01-01

    A detailed investigation of the initial film grown on mechanically polished Mg electrodes has been carried out by ex situ X-ray Photoelectron Spectroscopy (XPS) and in situ Photocurrent Spectroscopy (PCS), allowing to reach a detailed picture of the passive layer structure. The XPS data show that the films formed soon after mechanical treatment and immersion in aqueous electrolyte have a bilayer structure, consisting of an ultra-thin MgO inner layer (∼2.5 nm) and a Mg(OH) 2 external layer. The thickness of the Mg(OH) 2 layer is a function of immersion time and solution temperature. After mechanical treatment and immersion in aqueous solution at room temperature, the MgO/Mg(OH) 2 layer in some area of electrodes is so thin to allow an electron photoemission process from the Mg Fermi level to the electrolyte conduction band. Only internal photoemission processes are evidenced for Mg electrodes aged in NaOH at 80 deg. C, due the formation of a thicker Mg(OH) 2 layer. From anodic photocurrent spectra an optical band gap of ∼4.25 eV has been estimated for Mg(OH) 2 , lower with respect to the optical gap of the corresponding anhydrous counterpart

  12. An XPS [x-ray photoelectron spectroscopy] study of the sulfidation-regeneration cycle of a hydroprocessing catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Shang, D.Y.; Adnot, A.; Kaliaguine, S. (Laval Univ., Ste-Foy, PQ (Canada)); Chmielowiec, J. (Petro Canada Products Co., Mississauga, ON (Canada))

    1993-10-01

    The formation of sulfates in an industrial Ni-W hydroprocessing (HP) catalyst was investigated by x-ray photoelectron spectroscopy (XPS). A small fluidized bed test unit with on-line sampling device was constructed to simulate industrial sulfidation and oxyregeneration processes of HP catalysts. The results obtained show that the sulfates observed on the surface of sulfided catalysts are not formed during the sulfidation process. Two oxidation processes seem to be responsible for the formation of sulfates: one happens when the catalyst is exposed to air before it is properly cooled and the other is a slow conversion at ambient temperature. The two different processes might be associated to different sulfidic species formed during the sulfidation processes, with the sulfides in the bulk of catalyst particles being more easily oxidized than the ones on the external surface of the catalyst particles. The sulfate formed during the air oxidation of sulfided catalysts, as well as that after oxyregeneration, is not aluminum sulfate but nickel sulfate in both cases. XPS results also indicate that oxygenates in the feedstock are not directly involved in the sulfate formation. 18 refs., 9 figs., 6 tabs.

  13. The influence of oxygen adsorption on the NEXAFS and core-level XPS spectra of the C60 derivative PCBM

    International Nuclear Information System (INIS)

    Brumboiu, Iulia Emilia; Eriksson, Olle; Brena, Barbara; Ericsson, Leif; Hansson, Rickard; Moons, Ellen

    2015-01-01

    Fullerenes have been a main focus of scientific research since their discovery due to the interesting possible applications in various fields like organic photovoltaics (OPVs). In particular, the derivative [6,6]-phenyl-C 60 -butyric acid methyl ester (PCBM) is currently one of the most popular choices due to its higher solubility in organic solvents compared to unsubstituted C 60 . One of the central issues in the field of OPVs is device stability, since modules undergo deterioration (losses in efficiency, open circuit voltage, and short circuit current) during operation. In the case of fullerenes, several possibilities have been proposed, including dimerization, oxidation, and impurity related deterioration. We have studied by means of density functional theory the possibility of oxygen adsorption on the C 60 molecular moiety of PCBM. The aim is to provide guidelines for near edge X-ray absorption fine structure (NEXAFS) and X-ray photoelectron spectroscopy (XPS) measurements which can probe the presence of atomic or molecular oxygen on the fullerene cage. By analysing several configurations of PCBM with one or more adsorbed oxygen atoms, we show that a joint core level XPS and O1s NEXAFS investigation could be effectively used not only to confirm oxygen adsorption but also to pinpoint the bonding configuration and the nature of the adsorbate

  14. An AFM and XPS study of corrosion caused by micro-liquid of dilute sulfuric acid on stainless steel

    International Nuclear Information System (INIS)

    Wang Rongguang

    2004-01-01

    Micro-liquid of dilute sulfuric acid deposited on SUS304 steel surface were observed with the ac non-contact mode of an atomic force microscopy (AFM), and the detail of the corrosion process caused by them was investigated with the contact mode of the AFM, X-ray photoelectron spectroscopy (XPS) and wavelength dispersive X-ray spectroscopy (WDXS). As a result, even not applying bias voltages between the tip of the cantilever and the specimen, micro-liquid of sulfuric acid can be successfully imaged using the ac non-contact mode of AFM. Two shapes of micro-acid, i.e., micro-droplets and micro-films, were found to co-exist on the specimen surface. On areas covered by micro-films of acid, only small corrosion product particles appeared and no corrosion pits were found. Beneath micro-droplets, corrosion reaction continue to produce pits until they were all consumed to form a corrosion product (mainly iron oxides) with almost the same shape with the droplet. The total corrosion reaction time was speculated to be between 690 and 1500 ks. The corrosion product formed from micro-droplets was believed to be a process of accumulating small corrosion product particles from the liquid/substrate interface to the surface of the formerly produced corrosion product. The XPS and WDXS analysis also supports the above results

  15. Influence of oxygen incorporation on the defect structure of GaN microrods and nanowires. An XPS and CL study

    International Nuclear Information System (INIS)

    Guzmán, G; Herrera, M; Silva, R; Vásquez, G C; Maestre, D

    2016-01-01

    We report a cathodoluminescence (CL) and x-ray photoelectron spectroscopy (XPS) study of the influence of oxygen incorporation on the defect structure of GaN microrods and nanowires. The micro- and nanostructures were synthesized by a thermal evaporation method, which enables us to incorporate oxygen at different concentrations by varying the growth temperature. HR-TEM measurements revealed that oxygen generates stacking fault defects and edge dislocations along the GaN nanowires. Amorphous GaO x N y compounds were segregated on the surface of the nanowires. XPS, XRD and CL measurements suggests that the microrods and nanowires were composed of amorphous oxynitride compounds at their surface and GaN at their inner region. CL measurements revealed that the nanostructures generated an emission of 2.68 eV that increased in intensity proportionally to their oxygen content. We have attributed this emission to electronic transitions between donor substitutional-oxygen (O N ) and acceptor interstitial-oxygen (O i ) state levels. (paper)

  16. XPS\\KOUADIO KOUASSI.xps

    African Journals Online (AJOL)

    HP Pro 2000

    éclaircie dans les impénétrables régénérations de chêne. Dans la forêt tropicale guyanaise, Guitet et al. (2009) ont montré que l'application mixte des éclaircies sélective et systématique a permis une forte croissance en diamètre des tiges des ...

  17. CO dissociation and CO hydrogenation on smooth and ion-bombarded Pd(1 1 1): SFG and XPS spectroscopy at mbar pressures

    Science.gov (United States)

    Rupprechter, G.; Kaichev, V. V.; Unterhalt, H.; Morkel, M.; Bukhtiyarov, V. I.

    2004-07-01

    The CO dissociation probability on transition metals is often invoked to explain the product distribution (selectivity) of catalytic CO hydrogenation. Along these lines, we have investigated CO adsorption and dissociation on smooth and ion-bombarded Pd(1 1 1) at pressures up to 1 mbar using vibrational sum frequency generation (SFG) and X-ray photoelectron spectroscopy (XPS). Under high pressure, CO adsorbate structures were observed that were identical to high-coverage structures in UHV. On ion-bombarded surfaces an additional species was detected which was attributed to CO bridge bonded to defect (low-coordinated) sites. On both surfaces, no indications of CO dissociation were found even after hours of 0.1 mbar CO exposure. However, exposing CO/H 2 mixtures to ion-bombarded Pd(1 1 1) produced carbonaceous deposits suggesting CH xO species as precursors for CO bond cleavage and that the formation of CH xO is facilitated by surface defects. The relevance of the observations for CO hydrogenation on Pd catalysts is discussed.

  18. CO dissociation and CO hydrogenation on smooth and ion-bombarded Pd(1 1 1): SFG and XPS spectroscopy at mbar pressures

    Energy Technology Data Exchange (ETDEWEB)

    Rupprechter, G.; Kaichev, V.V.; Unterhalt, H.; Morkel, M.; Bukhtiyarov, V.I

    2004-07-31

    The CO dissociation probability on transition metals is often invoked to explain the product distribution (selectivity) of catalytic CO hydrogenation. Along these lines, we have investigated CO adsorption and dissociation on smooth and ion-bombarded Pd(1 1 1) at pressures up to 1 mbar using vibrational sum frequency generation (SFG) and X-ray photoelectron spectroscopy (XPS). Under high pressure, CO adsorbate structures were observed that were identical to high-coverage structures in UHV. On ion-bombarded surfaces an additional species was detected which was attributed to CO bridge bonded to defect (low-coordinated) sites. On both surfaces, no indications of CO dissociation were found even after hours of 0.1 mbar CO exposure. However, exposing CO/H{sub 2} mixtures to ion-bombarded Pd(1 1 1) produced carbonaceous deposits suggesting CH{sub x}O species as precursors for C---O bond cleavage and that the formation of CH{sub x}O is facilitated by surface defects. The relevance of the observations for CO hydrogenation on Pd catalysts is discussed.

  19. An XPS study of bromine in methanol etching and hydrogen peroxide passivation treatments for cadmium zinc telluride radiation detectors

    International Nuclear Information System (INIS)

    Babar, S.; Sellin, P.J.; Watts, J.F.; Baker, M.A.

    2013-01-01

    Highlights: ► CdZnTe single crystal etched in bromine-in-methanol and passivated in H 2 O 2 . ► XPS depth used to accurately determine enriched Te layer and TeO 2 thickness. ► For 0.2 and 2.0 (v/v) % bromine-in-methanol treatments, enriched Te layer thickness determined to be 1.3 and 1.8 nm, respectively. ► After passivation in 30 wt.% H 2 O 2 , the oxide thickness varies between 1.0 and 1.25 nm depending on the calculation method. - Abstract: The performance of single crystal CdZnTe radiation detectors is dependent on both the bulk and the surface properties of the material. After single crystal fabrication and mechanical polishing, modification of the surface to remove damage and reduce the surface leakage current is generally achieved through chemical etching followed by a passivation treatment. In this work, CdZnTe single crystals have been chemically etched using a bromine in methanol (BM) treatment. The BM concentrations employed were 0.2 and 2.0 (v/v) % and exposure times varied between 5 and 120 s. Angle resolved XPS and sputter depth profiling has been employed to characterize the surfaces for the different exposure conditions. A Te rich surface layer was formed for all exposures and the layer thickness was found to be independent of exposure time. The enriched Te layer thickness was accurately determined by calibrating the sputter rate against a CdTe layer of known thickness. For BM concentrations of 0.2 (v/v) % and 2 (v/v) %, the Te layer thickness was determined to be 1.3 ± 0.2 and 1.8 ± 0.2 nm, respectively. The BM etched surfaces have subsequently been passivated in a 30 wt.% H 2 O 2 solution employing exposure time of 15 s. The oxide layer thickness has been calculated using two standard XPS methodologies, based on the Beer–Lambert expression. The TeO 2 thickness calculated from ARXPS data are slightly higher than the thickness obtained by the simplified Beer–Lambert expression. For BM exposures of 30–120 s followed by a passivation

  20. The parallel processing of EGS4 code on distributed memory scalar parallel computer:Intel Paragon XP/S15-256

    Energy Technology Data Exchange (ETDEWEB)

    Takemiya, Hiroshi; Ohta, Hirofumi; Honma, Ichirou

    1996-03-01

    The parallelization of Electro-Magnetic Cascade Monte Carlo Simulation Code, EGS4 on distributed memory scalar parallel computer: Intel Paragon XP/S15-256 is described. EGS4 has the feature that calculation time for one incident particle is quite different from each other because of the dynamic generation of secondary particles and different behavior of each particle. Granularity for parallel processing, parallel programming model and the algorithm of parallel random number generation are discussed and two kinds of method, each of which allocates particles dynamically or statically, are used for the purpose of realizing high speed parallel processing of this code. Among four problems chosen for performance evaluation, the speedup factors for three problems have been attained to nearly 100 times with 128 processor. It has been found that when both the calculation time for each incident particles and its dispersion are large, it is preferable to use dynamic particle allocation method which can average the load for each processor. And it has also been found that when they are small, it is preferable to use static particle allocation method which reduces the communication overhead. Moreover, it is pointed out that to get the result accurately, it is necessary to use double precision variables in EGS4 code. Finally, the workflow of program parallelization is analyzed and tools for program parallelization through the experience of the EGS4 parallelization are discussed. (author).

  1. Quantitative analysis of Fe and Co in Co-substituted magnetite using XPS: The application of non-linear least squares fitting (NLLSF)

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Hongmei, E-mail: hmliu@gig.ac.cn [CAS Key Laboratory of Mineralogy and Metallogeny/Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, 510640 (China); Wei, Gaoling [Guangdong Key Laboratory of Agricultural Environment Pollution Integrated Control, Guangdong Institute of Eco-Environmental and Soil Sciences, Guangzhou, 510650 (China); Xu, Zhen [School of Materials Science and Engineering, Central South University, Changsha, 410012 (China); Liu, Peng; Li, Ying [CAS Key Laboratory of Mineralogy and Metallogeny/Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, 510640 (China); University of Chinese Academy of Sciences, Beijing, 100049 (China)

    2016-12-15

    Highlights: • XPS and Auger peak overlapping complicates Co-substituted magnetite quantification. • Disrurbance of Auger peaks was eliminated by non-linear least squares fitting. • Fitting greatly improved the accuracy of quantification for Co and Fe. • Catalytic activity of magnetite was enhanced with the increase of Co substitution. - Abstract: Quantitative analysis of Co and Fe using X-ray photoelectron spectroscopy (XPS) is of important for the evaluation of the catalytic ability of Co-substituted magnetite. However, the overlap of XPS peaks and Auger peaks for Co and Fe complicate quantification. In this study, non-linear least squares fitting (NLLSF) was used to calculate the relative Co and Fe contents of a series of synthesized Co-substituted magnetite samples with different Co doping levels. NLLSF separated the XPS peaks of Co 2p and Fe 2p from the Auger peaks of Fe and Co, respectively. Compared with a control group without fitting, the accuracy of quantification of Co and Fe was greatly improved after elimination by NLLSF of the disturbance of Auger peaks. A catalysis study confirmed that the catalytic activity of magnetite was enhanced with the increase of Co substitution. This study confirms the effectiveness and accuracy of the NLLSF method in XPS quantitative calculation of Fe and Co coexisting in a material.

  2. On-Surface Synthesis by Click Chemistry Investigated by STM and XPS

    DEFF Research Database (Denmark)

    Vadapoo, Sundar Raja

    2014-01-01

    Molecular synthesis is essential in the bottom-up approach of achieving highly stable nanostructures. On-surface synthesis is highly interesting from the basic science of view to improve the understanding of molecular behavior adsorbed on metal surfaces, and has potential applications such as mol......Molecular synthesis is essential in the bottom-up approach of achieving highly stable nanostructures. On-surface synthesis is highly interesting from the basic science of view to improve the understanding of molecular behavior adsorbed on metal surfaces, and has potential applications...... such as molecular electronics and surface functionalization. In this thesis, a well-defined click chemistry approach is followed, with the study of azide-alkyne cycloaddition on Cu(111) surface in UHV environment. A successful achievement of the click reaction product via on-surface synthesis has been shown, which...

  3. The 4s- and 4p- XPS spectra of Xe, XeF2 and XeF4

    International Nuclear Information System (INIS)

    Ohno, Masahide

    2003-01-01

    The 4s- and 4p- XPS spectra of Xe gas, XeF 2 molecule and XeF 4 molecule are calculated by an ab-initio atomic many-body theory. The 4s-peak and the prominent '4p'-peak are predicted well by the present theory. In XeF 2 and XeF 4 the spectral lines observed below the 4d-double ionization threshold are the 4d -2 4f multiplet states strongly perturbed by the interaction with the initial 4p 1/2 -hole state. They are very similar to the spectral lines which emerge with an increase in atomic number (e.g. Ba)

  4. Depth profile analysis of polymerized fluorine compound on photo-resist film with angle-resolved XPS

    International Nuclear Information System (INIS)

    Iijima, Yoshitoki; Kubota, Toshio; Oinaka, Syuhei

    2013-01-01

    Angle-resolved XPS (ARXPS) is an observation technique which is very effective in chemical depth analysis method less than photoelectron detected depth. For the analysis of depth profile, several analysis methods have been proposed to calculate the depth profile using the ARXPS method. The present report is the measurements of depth profile of the fluorine in a fluorine-containing photo-resist film using the ARXPS method and the depth profile of concentration have been successfully determined using the ARCtick 1.0 software. It has been observed that thickness of the fluorocarbon enriched surface layer of the photo-resist was 2.7 nm, and so that the convert of the ARXPS data from the angle profile to the depth profile was proved to be useful analysis method for the ultrathin layer depth. (author)

  5. Tracking the conversion of nitrogen during pyrolysis of antibiotic mycelial fermentation residues using XPS and TG-FTIR-MS technology.

    Science.gov (United States)

    Zhu, Xiangdong; Yang, Shijun; Wang, Liang; Liu, Yuchen; Qian, Feng; Yao, Wenqing; Zhang, Shicheng; Chen, Jianmin

    2016-04-01

    Antibiotic mycelial fermentation residues (AMFRs), which are emerging solid pollutants, have been recognized as hazardous waste in China since 2008. Nitrogen (N), which is an environmental sensitivity element, is largely retained in AMFR samples derived from fermentation substrates. Pyrolysis is a promising technology for the treatment of solid waste. However, the outcomes of N element during the pyrolysis of AMFRs are still unknown. In this study, the conversion of N element during the pyrolysis of AMFRs was tracked using XPS (X-ray photoelectron spectroscopy) and online TG-FTIR-MS (Thermogravimetry-Fourier transform infrared-Mass spectrometry) technology. In the AMFR sample, organic amine-N, pyrrolic-N, protein-N, pyridinic-N, was the main N-containing species. XPS results indicated that pyrrolic-N and pyridinic-N were retained in the AMFR-derived pyrolysis char. More stable species, such as N-oxide and quaternary-N, were also produced in the char. TG-FTIR-MS results indicated that NH3 and HCN were the main gaseous species, and their contents were closely related to the contents of amine-N and protein-N, and pyrrolic-N and pyridinic-N of AMFRs, respectively. Increases in heating rate enhanced the amounts of NH3 and HCN, but had less of an effect on the degradation degree of AMFRs. N-containing organic compounds, including amine-N, nitrile-N and heterocyclic-N, were discerned from the AMFR pyrolysis process. Their release range was extended with increasing of heating rate and carbon content of AMFR sample. This work will help to take appropriate measure to reduce secondary pollution from the treatment of AMFRs. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. XPS study of the Ln 5p,4f-electronic states of lanthanides in Ln2O3

    International Nuclear Information System (INIS)

    Teterin, Yu.A.; Teterin, A.Yu.; Utkin, I.O.; Ryzhkov, M.V.

    2004-01-01

    The present work analyses the fine structure of the low binding energy (E b , 0-50 eV) X-ray photoelectron spectra XPS of lanthanide (La through Lu excepted for Pm) oxides, and compares it with the non-relativistic X α -discrete variation calculation results for the clusters reflecting the close environment of lanthanides in oxides. The obtained results show that the Ln 4f n -electrons of lanthanides in oxides by their spectral parameters have much in common with the M 3d-electrons in oxides of the 3d-transition metals. According to these data, the Ln 4f shell of lanthanides is rather outer and can participate in the formation of molecular orbitals in compounds. The XPS data at least do not contradict the theoretical suggestion about the significant participation of the Ln 4f-electrons in formation of the molecular orbitals in the studied materials. The spectra in the Ln 5p-O 2s binding energy region of the studied lanthanide oxides were found to exhibit the complicated structure instead of separated peaks due to the electrons of the Ln 5p 3/2,5/2 and O 2s atomic shells. Taking into account the energy differences between the inner (Ln 3d) and outer (Ln 5p) electronic shells for some metallic lanthanides and their oxides, the Ln 5p atomic shells were shown to participate in the formation of the inner valence molecular orbitals (IVMO). That agrees qualitatively with the calculation results

  7. H:\\PMKER 25(2)\\PDF 25(2)\\BAN KOFFI.xps

    African Journals Online (AJOL)

    AISA

    L.R., Montville T.J. (Eds.). Food Microbiology-. Fundamentals and frontiers. ASM Press,. Washington, D.C., pp. 721 -733. Timbie D. J., Sechrist L. and P. G. Keeney. 1978. Application of high pressure liquid chromatography to the study of variables affecting theobromine and caffeine concentrations in cocoa beans. J Food Sci.

  8. Multicenter study on costs associated with two surgical procedures: GreenLight XPS 180 W versus the gold standard transurethral resection of the prostate.

    Science.gov (United States)

    Benejam-Gual, J M; Sanz-Granda, A; Budía, A; Extramiana, J; Capitán, C

    2014-01-01

    To analyze the costs associated with two surgical procedures for lower urinary tract symptoms secondary to benign prostatic hyperplasia: GreenLight XPS 180¦W versus the gold standard transurethral resection of the prostate. A multicenter, retrospective cost study was carried out from the National Health Service perspective, over a 3-month time period. Costs were broken down into pre-surgical, surgical and post-surgical phases. Data were extracted from records of patients operated sequentially, with IPSS=15, Qmax=15 mL/seg and a prostate volume of 40-80mL, adding only direct healthcare costs (€, 2013) associated with the procedure and management of complications. A total of 79 patients sequentially underwent GL XPS (n: 39) or TURP (n: 40) between July and October, 2013. Clinical outcomes were similar (94.9% and 92.5%, GL XPS and TURP, respectively) without significant differences (P=.67). The average direct cost per patient was reduced by €114 in GL XPS versus TURP patients; the cost was higher in the surgical phase with GL XPS (difference: €1,209; P<.001) but was lower in the post-surgical phase (difference: €-1,351; P<.001). The GreenLight XPS 180-W laser system is associated with a reduction in costs with respect to transurethral resection of prostate in the surgical treatment of LUTS secondary to PBH. This reduction is due to a shorter inpatient length of stay that offsets the cost of the new technology. Copyright © 2013 AEU. Published by Elsevier Espana. All rights reserved.

  9. XPS studies of Mg doped GDC (Ce0.8Gd0.2O2-δ) for IT-SOFC

    Science.gov (United States)

    Tyagi, Deepak; Rao, P. Koteswara; Wani, B. N.

    2018-04-01

    Fuel Cells have gained much attention as efficient and environment friendly device for both stationary as well as mobile applications. For intermediate temperature SOFC (IT-SOFC), ceria based electrolytes are the most promising one, due to their higher ionic conductivity at relatively lower temperatures. Gd doped ceria is reported to be having the highest ionic conductivity. In the present work, Mg is codoped along with Gd and the electronic structure of the constituents is studied by XPS. XPS confirm that the Cerium is present in +4 oxidation state only which indicates that electronic conduction can be completely avoided.

  10. Study by X-ray photoelectron spectroscopy (XPS) and radiochemistry (Cl36) of the interaction of chloride ions with a passive film formed on nickel

    International Nuclear Information System (INIS)

    Herbelin, Jean-Marc

    1990-01-01

    This research thesis reports the study of the influence of chlorides on nickel passivation by using a radiochemical method based on the use of the Cl 36 isotope and the X-ray photoelectron spectroscopy (XPS). The first one allows the in-situ determination of the adsorption of chlorides on the surface, or their inclusion in surface films during the electrochemical treatment. The XPS analysis allows the characterization of modifications induced by chlorides in passive films. The obtained results allow a better understanding in the interpretation of the mechanisms of corrosion induced by chloride ions [fr

  11. Radiation-induced defects in chalcogenide glasses characterized by combined optical spectroscopy, XPS and PALS methods

    International Nuclear Information System (INIS)

    Shpotyuk, O.; Kovalskiy, A.; Jain, H.; Golovchak, R.; Zurawska, A.

    2007-01-01

    Temperature-dependent optical absorption spectroscopy, high-resolution X-ray photoelectron spectroscopy and positron annihilation lifetimes spectroscopy are utilized to understand radiation-induced changes in Ge-Sb-S chalcogenide glasses. Theoretically predicted topological scheme of γ-induced coordination defect formation in stoichiometric Ge 23.5 Sb 11.8 S 64.7 glass composition is supported by these measurements. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  12. Surface chemistry changes of weathered HDPE/wood-flour composites studied by XPS and FTIR spectroscopy

    Science.gov (United States)

    Nicole M. Stark; Laurent M. Matuana

    2004-01-01

    The use of wood-derived fillers by the thermoplastic industry has been growing, fueled in part by the use of wood-fiber–thermoplastic composites by the construction industry. As a result, the durability of wood-fiber– thermoplastic composites after ultraviolet exposure has become a concern. Samples of 100% high-density polyethylene (HDPE) and HDPE filled with 50% wood-...

  13. XPS: A multi-channel preamplifier-shaper IC for X-ray spectroscopy

    International Nuclear Information System (INIS)

    Krieger, B.; Kipnis, I.; Ludewigt, B.A.

    1997-11-01

    An integrated circuit featuring 48 channels of charge-sensitive preamplifiers followed by variable-gain pulse shaping amplifiers is being developed as part of an x-ray spectrometer with a highly segmented detector to handle high fluxes in synchrotron experiments. Such detector systems can provide excellent energy resolution combined with one-dimensional spatial information. The IC combines many basic spectroscopy amplifier functions with a low-noise preamplifier section to produce a unique circuit capable of driving conventional ADC modules directly. An important feature of the design is the novel CR-RC 2 pulse shaper. In this section, high-linearity transconductor circuits are required in order to provide a broad range of continuously variable peaking times while still maintaining the linearity and noise performance necessary for x-ray spectroscopy. Reported here are first measurements made on the performance of a 16-channel prototype integrated circuit. At present, the preamplifier-shaper circuit achieves an equivalent input noise of 26 electrons rms at 2 micros peaking time with a 0.2 pF external capacitor, which is similar to the capacitance of a single detector element. The design was fabricated in standard 1.2 microm CMOS technology

  14. XPS analysis of supported catalysts prepared in water-in-oil microemulsion system

    International Nuclear Information System (INIS)

    Mohd Ambar Yarmo; Wong Hoi Jin; Tan Chew Khim; Anita Ramli; Shahidan Radiman

    2002-01-01

    Catalysts supported on γ-alumina prepared by water-in-oil microemulsion were studied by X-ray photoelectron spectroscopy for comparison with catalysts prepared by wet impregnation. Comparable shifts to higher binding energies indicated a metal-support interaction where metal obtained via microemulsion is very small in size and highly dispersed. The positive binding energy shifts could be explained from a net unit positive charge remaining on the cluster in the photoemission final state in addition to the metallic screening from a redistribution of states within the bands. (Author)

  15. Radiation-induced defects in chalcogenide glasses characterized by combined optical spectroscopy, XPS and PALS methods

    Energy Technology Data Exchange (ETDEWEB)

    Shpotyuk, O. [Institute of Physics of Jan Dlugosz University, 13/15 al. Armii Krajowej, Czestochowa 42201 (Poland); Lehigh University, 5 East Packer Avenue, Bethlehem, PA 18015-3195 (United States); Lviv Institute of Materials of SRC ' ' Carat' ' , 202, Stryjska str., 79031 Lviv (Ukraine); Kovalskiy, A.; Jain, H. [Lehigh University, 5 East Packer Avenue, Bethlehem, PA 18015-3195 (United States); Golovchak, R. [Lehigh University, 5 East Packer Avenue, Bethlehem, PA 18015-3195 (United States); Lviv Institute of Materials of SRC ' ' Carat' ' , 202, Stryjska str., 79031 Lviv (Ukraine); Zurawska, A. [Opole University of Technology, 75, Ozimska str., Opole 45370 (Poland)

    2007-03-15

    Temperature-dependent optical absorption spectroscopy, high-resolution X-ray photoelectron spectroscopy and positron annihilation lifetimes spectroscopy are utilized to understand radiation-induced changes in Ge-Sb-S chalcogenide glasses. Theoretically predicted topological scheme of {gamma}-induced coordination defect formation in stoichiometric Ge{sub 23.5}Sb{sub 11.8}S{sub 64.7} glass composition is supported by these measurements. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. Gettering effects in RAD polysilicon ribbons: An XPS/AES study

    Energy Technology Data Exchange (ETDEWEB)

    Amarray, E.; Deville, J.P.; Quesada, J.

    1987-03-01

    Evidence for gettering effects during the various heat treatments applied to RAD ribbons were investigated with surface analysis methods. These heat treatments occur either during the burning-off process of the carbon support or during the POCl/sub 3/ diffusion, and transport metallic impurities near the surface of the sample. Oxidation of clean silicon surfaces, cleaved either in air or ultra-high vacuum, has shown that the same metallic impurities are brought near the surface by this treatment alone. It is thus suggested that controlled oxidations and heat treatments can be used to improve the electrical properties of polysilicon, and especially of ribbons.

  17. Evaluation of Surface Cleaning Procedures for CTGS Substrates for SAW Technology with XPS

    Directory of Open Access Journals (Sweden)

    Erik Brachmann

    2017-11-01

    Full Text Available A highly efficient and reproducible cleaning procedure of piezoelectric substrates is essential in surface acoustic waves (SAW technology to fabricate high-quality SAW devices, especially for new applications such SAW sensors wherein new materials for piezoelectric substrates and interdigital transducers are used. Therefore, the development and critical evaluation of cleaning procedures for each material system that is under consideration becomes crucial. Contaminants like particles or the presence of organic/inorganic material on the substrate can dramatically influence and alter the properties of the thin film substrate composite, such as wettability, film adhesion, film texture, and so on. In this article, focus is given to different cleaning processes like SC-1 and SC-2, UV-ozone treatment, as well as cleaning by first-contact polymer Opticlean, which are applied for removal of contaminants from the piezoelectric substrate Ca 3 TaGa 3 Si 2 O 14 . By means of X-ray photoelectron spectroscopy, the presence of the most critical contaminants such as carbon, sodium, and iron removed through different cleaning procedures were studied and significant differences were observed between the outcomes of these procedures. Based on these results, a two-step cleaning process, combining SC-1 at a reduced temperature at 30 ∘ C instead of 80 ∘ C and a subsequent UV-ozone cleaning directly prior to deposition of the metallization, is suggested to achieve the lowest residual contamination level.

  18. The XPS study of the structure of uranium-containing ceramics

    Directory of Open Access Journals (Sweden)

    Teterin Anton Yu.

    2010-01-01

    Full Text Available The samples of the (Ca0.5GdU0.5Zr2O7 and (Ca0.5GdU0.5(ZrTiO7 ceramics with the fluorite and pyrochlore structures used as matrixes for the long-lived high-level radioactive waste disposal were studied with the X-ray photoelectron spectroscopy method. On the basis of the X-ray photoelectron spectroscopy parameters of the outer and core electrons from the binding energy range of 0-1250 eV the oxidation states of the included metal ions were determined, the quantitative elemental and ionic analysis was done, and the orderliness (monophaseness was evaluated. The obtained data agree with the X-ray diffraction and the scanning electron microscopy results.

  19. XPS and Ag L3-edge XANES characterization of silver and silver-gold sulfoselenides

    Science.gov (United States)

    Mikhlin, Yuri L.; Pal'yanova, Galina A.; Tomashevich, Yevgeny V.; Vishnyakova, Elena A.; Vorobyev, Sergey A.; Kokh, Konstantin A.

    2018-05-01

    Gold and silver sulfoselenides are of interest as materials with high ionic conductivity and promising magnetoresistive, thermoelectric, optical, and other physico-chemical properties, which are strongly dependent on composition and structure. Here, we applied X-ray photoelectron spectroscopy and Ag L3 X-ray absorption near-edge structure (XANES) to study the electronic structures of low-temperature compounds and solid solutions Ag2SxSe1-x (0 compounds; in particular, the Ag L3-edge peak is about 35% lower for AgAuS relative to Ag2S. At the same time, the Au 4f binding energy and, therefore, charge at Au(I) sites increase with increasing S content due to the transfer of electron density from Au to Ag atoms. It was concluded that the effects mainly originate from shortening of the metal-chalcogen and especially the Ausbnd Ag interatomic distances in substances having similar coordination geometry.

  20. XPS study of graphene oxide reduction induced by (100) and (111)-oriented Si substrates

    Science.gov (United States)

    Priante, F.; Salim, M.; Ottaviano, L.; Perrozzi, F.

    2018-02-01

    The reduction of graphene oxide (GO) has been extensively studied in literature in order to let GO partially recover the properties of graphene. Most of the techniques proposed to reduce GO are based on high temperature annealing or chemical reduction. A new procedure, based on the direct reduction of GO by etched Si substrate, was recently proposed in literature. In the present work, we accurately investigated the Si-GO interaction with x-ray photoelectron spectroscopy. In order to avoid external substrate oxidation factors we used EtOH as the GO solvent instead of water, and thermal annealing was carried out in UHV. We investigated the effect of Si(100), Si(111) and Au substrates on GO, to probe the role played by both the substrate composition and substrate orientation during the reduction process. A similar degree of GO reduction was observed for all samples but only after thermal annealing, ruling out the direct reduction effect of the substrate.

  1. Measurements of Chlorine by XPS and SIMS in Nuclear-Grade Graphite. Effect of Treatment by UV, Heat and Moisture

    International Nuclear Information System (INIS)

    Grossiord, C.; Amalric, J.; Rahmani, L.

    2016-01-01

    Pieces of historical nuclear-grade graphite from the same block were submitted to a treatment involving soft or hard UV and heating in moist air. XPS investigations before treatment have shown that – at the geometric surface at least – chlorine binds more commonly by covalent (30 to 100% depending on spots) than ionic bonds. After treatment, bond types are more balanced, though hardly more uniform. Shifts of the ionic peak indicating an oxidised bond were not found. Surface chlorine was measured up to 0.04% atomic. Treatment by hard UV and heating in moist air for 1 ½ hours up to 122°C led to a decrease of surface chlorine by a factor of 2 as measured by ToF and XPS, helped by an etching technique that ensured the accurate positioning of the spots under analysis. Treatment for 8 hours up to 151°C resulted in a decrease of the ToF Cl/ 13 C signal for surface chlorine from 0.73 to 0.20 and of the atomic fraction from 0.02% to 0% as measured by XPS. SIMS investigations reveal that in the first 6 μm from the geometric surface, chlorine, hydrogen and oxygen have a decreasing profile suggestive of diffusion from the surface. In the vicinity to the surface the amounts of all three elements are much greater than in the bulk, possibly due to the availability of dangling bonds. It is speculated that when these are not saturated, back diffusion from the bulk under treatment may increase the quantity of surface chlorine. Treatment in moist air by hard UV for to 1 ½ hours has no marked effect on chlorine in the bulk, although it alters the quantities of hydrogen and oxygen. Treatment for 8 hours decreases chlorine by a factor of about 5 throughout the analysed depth of 6 μm and possibly farther to 15 μm, suggesting its diffusivity to be at least an order greater than 3.10 -16m 2 /s and possibly than 2.10 -15 m²/s, although a range of values is expected owing to the diverse tortuosity and constrictivity of pores. Ratios of hydrogen to oxygen and of chlorine to

  2. Extended study on oxidation behaviors of UN0.68 and UN1.66 by XPS

    Science.gov (United States)

    Luo, Lizhu; Hu, Yin; Pan, Qifa; Long, Zhong; Lu, Lei; Liu, Kezhao; Wang, Xiaolin

    2018-04-01

    The surface oxidation behaviors of UN0.68 and UN1.66 thin films are investigated by X-ray photoelectron spectroscopy (XPS), and the traditional U4f/N1s, O1s, valence band spectra as well as the unconventional U4d and U5d spectra are collected for the understanding of their oxidation behavior in-depth. Similar asymmetrical peak shape of the U4f spectra to uranium is observed for both uranium nitrides, despite of a slight shift to higher energy side for UN1.66 clean surface. However, significant difference among the corresponding spectra of UN0.68 and UN1.66 during oxidation reveals the distinctive properties of each own. The coexistence of UO2-x, UO2 and UO2-x.Ny on UN0.68 surface results in the peculiar features of U4f spectra as well as the others within the XPS energy scale, where peaks of the oxidized species firstly shift to higher energy side compared to the clean surface, and then return closely towards those of stoichiometric UO2. For UN1.66, the generation of U-N-O ternary compounds on the surface is identified with the symmetrical U4f peaks at 379.9eV and 390.8 eV, which locate intermediate between UO2 and UN1.66, and gradually expanding to higher energy side during the progressive oxidation. Furthermore, the formation of N-O species on UN1.66 surface is also detected as an oxidation product. The metallic character of UN1.66 is identified by the intense signal at Fermi level, which is greatly suppressed by the increasing oxygen exposure and implies the weakening metallic properties of the as-generated U-N-O compounds. Higher uranium oxides, such as UO3 and U4O9, are deduced to be the final oxidation products, and a multistage mechanism for UN1.66 following the exposure to oxygen is discussed.

  3. XPS Investigation of ceramic matrixes for disposal of long-living radioactive waste products

    Directory of Open Access Journals (Sweden)

    Teterin Yury A.

    2004-01-01

    Full Text Available The synthesis of ceramic matrixes for the long-term storage of highly active radionuclide wastes and determination of physical and chemical forms of radionuclides in them is one of the important problems in radioecology. It enables to create purpose fully materials for the long-term storage of radionuclides. In the present work the samples of ceramics [CaCe0.9Ti2O6.8(I and CaCeTi2O7(II}] formed under various conditions were investigated with the X-ray photo electron spectroscopy. It is necessary for synthesis of ceramic matrixes, for the disposal of the plutonium and others tetravalent actinides. A technique was developed for the determination of cerium oxidation state (Ce3+ and Ce4+ on the basis of the X-ray photo electron spectroscopy spectral structure characteristics. It was established that the sample (I formed at 300 MPa and T = 1400 °C in the air atmosphere contained on the surface two types of cerium ions in the ratio – 63 atomic % of Ce3+ and 37 atomic % of Ce4+, and the sample (II formed at 300 MPa and T= 1300 °C in the oxygen atmosphere contained on its surface two types of cerium ions also, but in the ratio – 36 atomic % of Ce3+ and 64 atomic % of Ce4+. It was established that on the surface of the studied ceramics carbonates of calcium and/or cerium could be formed under influence of the environment that leads to the destruction of ceramics.

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

    Science.gov (United States)

    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.

  5. On the nature of oxygen-containing surface groups on carbon nanofibers and their role for platinum deposition—an xps and titration study

    NARCIS (Netherlands)

    Plomp, A.J.; Su, D.S.; de Jong, K.P.; Bitter, J.H.

    2009-01-01

    XPS and acid−base titrations were used to investigate the nature and stability of oxygen-containing surface groups on carbon nanofibers (CNF) and platinum-containing CNF. During heat treatments in inert atmosphere at 973 K all acidic (carboxylic) oxygen surface groups were removed for CNF.

  6. Assessment of the surface chemistry of carbon blacks by TGA-MS, XPS and inverse gas chromatography using statistical chemometric analysis

    International Nuclear Information System (INIS)

    Strzemiecka, Beata; Voelkel, Adam; Donate-Robles, Jessica; Martín-Martínez, José Miguel

    2014-01-01

    Highlights: • Carbon blacks with lower specific surface area had basic character (electron donor) due to C=O and C-O groups. • Carbon blacks with higher specific surface area had acidic character (acceptor electron) due to OH groups. • Total surface energy and its dispersive component of carbon blacks increased by increasing their specific surface area. (table) - Abstract: Four carbon blacks with different specific surface areas and surface chemistries (C32, C71, C159 and C178) were analyzed by transmission electron microscopy (TEM) and nitrogen adsorption isotherms at 77 K. Their surface chemistries were analyzed by X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis coupled with mass spectrometry (TGA-MS) and inverse gas chromatography (IGC). The carbon blacks contained 2.7–5.8 wt% volatiles corresponding to -OH, C-O, C=O and COO groups. The surface chemistry parameters obtained with the different experimental techniques were inter-related by using chemometric statistical analysis tools. The application of this methodology showed that the carbon blacks with lower specific surface area (C32 and C71) had basic character (electron donor) mainly due to C=O and C-O groups, whereas the carbon black with the highest specific surface area (C178) showed acidic character (acceptor electron) due to its high content of OH groups. Moreover, the total surface energy and the dispersive component of the surface energy of the carbon blacks increased with the increase of their specific surface area. In general the specific interactions of the carbon blacks also increased with the increase of their specific surface area although C71 is exceptional due to higher oxygen content corresponding to C-O groups

  7. Ageing of plasma-mediated coatings with embedded silver nanoparticles on stainless steel: An XPS and ToF-SIMS investigation

    Science.gov (United States)

    Zanna, S.; Saulou, C.; Mercier-Bonin, M.; Despax, B.; Raynaud, P.; Seyeux, A.; Marcus, P.

    2010-09-01

    Nanocomposite thin films (˜170 nm), composed of silver nanoparticles enclosed in an organosilicon matrix, were deposited onto stainless steel, with the aim of preventing biofilm formation. The film deposition was carried out under cold plasma conditions, combining radiofrequency (RF) glow discharge fed with argon and hexamethyldisiloxane and simultaneous silver sputtering. XPS and ToF-SIMS were used to characterize Ag-organosilicon films in native form and after ageing in saline solution (NaCl 0.15 M), in order to further correlate their lifetime with their anti-fouling properties. Two coatings with significantly different silver contents (7.5% and 20.3%) were tested. Surface analysis confirmed the presence of metallic silver in the pristine coating and revealed significant modifications after immersion in the saline solution. Two different ageing mechanisms were observed, depending on the initial silver concentration in the film. For the sample exhibiting the low silver content (7.5%), the metal amount decreased at the surface in contact with the solution, due to the release of silver from the coating. As a result, after a 2-day exposure, silver nanoparticles located at the extreme surface were entirely released, whereas silver is still present in the inner part of the film. The coating thickness was not modified during ageing. In contrast, for the high silver content film (20.3%), the thickness decreased with immersion time, due to significant silver release and matrix erosion, assigned to a percolation-like effect. However, after 18 days of immersion, the delamination process stopped and a thin strongly bounded layer remained on the stainless steel surface.

  8. X-ray photoemission spectroscopy (XPS) and extended x-ray absorption fine structure (EXAFS) studies of silicate based glasses

    International Nuclear Information System (INIS)

    Karim, D.; Lam, D.J.

    1979-01-01

    The application of the x-ray photoemission spectroscopy (XPS) technique to study the electronic structure and bonding of heavy metal oxides in alkali- and alkali-earth-silicate glasses had been demonstrated. The bonding characteristics of the iron oxide and uranium oxide in sodium silicate glasses were deduced from the changes in the oxygen 1s levels and the heavy metal core levels. It is reasonable to expect that the effect of leaching on the heavy metal ions can be monitored using the appropriate core levels of these ions. To study the effect of leaching on the glass forming network, the valence band structure of the bridging and nonbridging oxygens in sodium silicate glasses were investigated. The measurement of extended x-ray absorption fine-structure (EXAFS) is a relatively new analytical technique for obtaining short range (<5 A) structural information around atoms of a selected species in both solid and fluid systems. Experiments have recently begun to establish the feasibility of using EXAFS to study the bonding of actinides in silicate glasses. Because of the ability of EXAFS to yield specific structural data even in complex multicomponent systems, it could prove to be an invaluable tool in understanding glass structure

  9. Effect of laser irradiation on the structure and valence states of copper in Cu-phosphate glass by XPS studies

    International Nuclear Information System (INIS)

    Khattak, G.D.; Mekki, A.; Gondal, M.A.

    2010-01-01

    The effect of laser irradiation using three different wavelengths (IR, visible and UV) generated from Nd:YAG laser on the local glass structure as well as on the valence state of the copper ions in copper phosphate glass containing CuO with the nominal composition 0.30(CuO)-(0.70)(P 2 O 5 ), has been investigated by X-ray photoelectron spectroscopy (XPS). The presence of asymmetry and satellite peaks in the Cu 2p spectrum for the unirradiated sample is an indication of the presence of two different valence states, Cu 2+ and Cu + . Hence, the Cu 2p 3/2 spectrum was fitted to two Gaussian-Lorentzian peaks and the corresponding ratio, Cu 2+ /Cu total , determined from these relative areas clearly shows that copper ions exist predominately (>86%) in the Cu 2+ state for the unirradiated glass sample under investigation. For the irradiated samples the symmetry and the absence of satellite peaks in the Cu 2p spectra indicate the existence of the copper ions mostly in Cu + state. The O 1s spectra show slight asymmetry for the irradiated as well as unirradiated glass samples which result from two contributions, one from the presence of oxygen atoms in the P-O-P environment (bridging oxygen BO) and the other from oxygen in an P-O-Cu and P=O environment (non-bridging oxygen NBO). The ratio of NBO to total oxygen was found to increase with laser power.

  10. XPS study of the ultrathin a-C:H films deposited onto ion beam nitrided AISI 316 steel

    International Nuclear Information System (INIS)

    Meskinis, S.; Andrulevicius, M.; Kopustinskas, V.; Tamulevicius, S.

    2005-01-01

    Effects of the steel surface treatment by nitrogen ion beam and subsequent deposition of the diamond-like carbon (hydrogenated amorphous carbon (a-C:H) and nitrogen doped hydrogenated amorphous carbon (a-CN x :H)) films were investigated by means of the X-ray photoelectron spectroscopy (XPS). Experimental results show that nitrogen ion beam treatment of the AISI 316 steel surface even at room temperature results in the formation of the Cr and Fe nitrides. Replacement of the respective metal oxides by the nitrides takes place. Formation of the C-N bonds was observed for both ultrathin a-C:H and ultrathin a-CN x :H layers deposited onto the nitrided steel. Some Fe and/or Cr nitrides still were presented at the interface after the film deposition, too. Increased adhesion between the steel substrate and hydrogenated amorphous carbon layer after the ion beam nitridation was explained by three main factors. The first two is steel surface deoxidisation/passivation by nitrogen as a result of the ion beam treatment. The third one is carbon nitride formation at the nitrided steel-hydrogenated amorphous carbon (or a-CN x :H) film interface

  11. XPS characterisation of in situ treated lanthanum oxide and hydroxide using tailored charge referencing and peak fitting procedures

    International Nuclear Information System (INIS)

    Sunding, M.F.; Hadidi, K.; Diplas, S.; Lovvik, O.M.; Norby, T.E.; Gunnaes, A.E.

    2011-01-01

    Highlights: → Gold particles deposited in vacuum as energy reference for insulating samples in XPS. → Separation of La 3d and MNN peaks in XP spectra acquired with Al Kα radiation. → We describe the spectral differences between lanthanum oxide and lanthanum hydroxide. → A doublet in O 1s of La 2 O 3 is ascribed to two distinct oxygen sites in the crystal. - Abstract: A technique is described for deposition of gold nanoparticles under vacuum, enabling consistent energy referencing of X-ray photoelectron spectra obtained from lanthanum hydroxide La(OH) 3 and in situ treated lanthanum oxide La 2 O 3 powders. A method is also presented for the separation of the overlapping lanthanum 3d and MNN peaks in X-ray photoelectron spectra acquired with Al Kα radiation. The lower satellite intensity in La(OH) 3 compared to La 2 O 3 is related to the higher ionicity of the La-O bond in the former compared to the latter compound. The presence of an additional peak in the valence band spectrum of the hydroxide compared to the oxide is attributed to the O-H bond as indicated by density functional theory based calculations. A doublet in the O 1s peak of lanthanum oxide is associated to the presence of two distinct oxygen sites in the crystal structure of this compound.

  12. XPS characterisation of in situ treated lanthanum oxide and hydroxide using tailored charge referencing and peak fitting procedures

    Energy Technology Data Exchange (ETDEWEB)

    Sunding, M.F., E-mail: m.f.sunding@fys.uio.no [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway); Hadidi, K. [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway); Diplas, S. [Department of Chemistry and Centre for Material Science and Nanotechnology (SMN), University of Oslo, P.O. Box 1033 Blindern, NO-0315 Oslo (Norway); SINTEF Materials and Chemistry, P.O. Box 124 Blindern, NO-0314 Oslo (Norway); Lovvik, O.M. [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway); SINTEF Materials and Chemistry, P.O. Box 124 Blindern, NO-0314 Oslo (Norway); Norby, T.E. [Department of Chemistry and Centre for Material Science and Nanotechnology (SMN), University of Oslo, P.O. Box 1033 Blindern, NO-0315 Oslo (Norway); Gunnaes, A.E. [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway)

    2011-07-15

    Highlights: {yields} Gold particles deposited in vacuum as energy reference for insulating samples in XPS. {yields} Separation of La 3d and MNN peaks in XP spectra acquired with Al K{alpha} radiation. {yields} We describe the spectral differences between lanthanum oxide and lanthanum hydroxide. {yields} A doublet in O 1s of La{sub 2}O{sub 3} is ascribed to two distinct oxygen sites in the crystal. - Abstract: A technique is described for deposition of gold nanoparticles under vacuum, enabling consistent energy referencing of X-ray photoelectron spectra obtained from lanthanum hydroxide La(OH){sub 3} and in situ treated lanthanum oxide La{sub 2}O{sub 3} powders. A method is also presented for the separation of the overlapping lanthanum 3d and MNN peaks in X-ray photoelectron spectra acquired with Al K{alpha} radiation. The lower satellite intensity in La(OH){sub 3} compared to La{sub 2}O{sub 3} is related to the higher ionicity of the La-O bond in the former compared to the latter compound. The presence of an additional peak in the valence band spectrum of the hydroxide compared to the oxide is attributed to the O-H bond as indicated by density functional theory based calculations. A doublet in the O 1s peak of lanthanum oxide is associated to the presence of two distinct oxygen sites in the crystal structure of this compound.

  13. Ellipsometry and XPS comparative studies of thermal and plasma enhanced atomic layer deposited Al2O3-films

    Directory of Open Access Journals (Sweden)

    Jörg Haeberle

    2013-11-01

    Full Text Available We report on results on the preparation of thin (2O3 films on silicon substrates using thermal atomic layer deposition (T-ALD and plasma enhanced atomic layer deposition (PE-ALD in the SENTECH SI ALD LL system. The T-ALD Al2O3 layers were deposited at 200 °C, for the PE-ALD films we varied the substrate temperature range between room temperature (rt and 200 °C. We show data from spectroscopic ellipsometry (thickness, refractive index, growth rate over 4” wafers and correlate them to X-ray photoelectron spectroscopy (XPS results. The 200 °C T-ALD and PE-ALD processes yield films with similar refractive indices and with oxygen to aluminum elemental ratios very close to the stoichiometric value of 1.5. However, in both also fragments of the precursor are integrated into the film. The PE-ALD films show an increased growth rate and lower carbon contaminations. Reducing the deposition temperature down to rt leads to a higher content of carbon and CH-species. We also find a decrease of the refractive index and of the oxygen to aluminum elemental ratio as well as an increase of the growth rate whereas the homogeneity of the film growth is not influenced significantly. Initial state energy shifts in all PE-ALD samples are observed which we attribute to a net negative charge within the films.

  14. Corrosion investigation of fire-gilded bronze involving high surface resolution spectroscopic imaging

    International Nuclear Information System (INIS)

    Masi, G.; Chiavari, C.; Avila, J.; Esvan, J.; Raffo, S.; Bignozzi, M.C.; Asensio, M.C.; Robbiola, L.

    2016-01-01

    Graphical abstract: - Highlights: • Fire-gilded bronze prepared by ancient methods (Au–Hg layer on Cu–Sn–Zn–Pb–Sb). • Heating during gilding induces Sn and Znenrichment in the top part of the gilded layer. • SR-HRPES mapping of corrosion craters (cross-section) after accelerated ageing. • Selective dissolution of Cu and Zn in the craters induces Sn species enrichment. • The main species in the craters are related to hydroxi-oxide compounds. - Abstract: Gilded bronzes are often affected by severe corrosion, due to defects in the Au layer and Au/Cu alloy galvanic coupling, stimulated by large cathodic area of the gilded layer. Galvanic corrosion, triggered by gilding defects, leads to products growth at the Au/bronze interface, inducing blistering or break-up of the Au layer. In this context, fire-gilded bronze replicas prepared by ancient methods (use of spreadable Au–Hg paste) was specifically characterised by compiling complementary spectroscopic and imaging information before/after accelerated ageing with synthetic rain. Fire-gilded bronze samples were chemically imaged in cross-section at nano-metric scale (<200 nm) using high energy and lateral resolution synchrotron radiation photoemission (HR-SRPES) of core levels and valence band after conventional characterisation of the samples by Glow Discharge optical Emission Spectroscopy (GD-OES) and conventional X-ray photoelectron spectroscopy (XPS). We have found a net surface enrichment in Zn and Sn after fire-gilding and presence of metallic Hg, Pb and Cu within the Au layer. Moreover, the composition distribution of the elements together with their oxidation has been determined. It was also revealed that metallic phases including Hg and Pb remain in the gilding after corrosion. Moreover, selective dissolution of Zn and Cu occurs in the crater due to galvanic coupling, which locally induces relative Sn species enrichment (decuprification). The feasibility advantages and disadvantages of

  15. Corrosion investigation of fire-gilded bronze involving high surface resolution spectroscopic imaging

    Energy Technology Data Exchange (ETDEWEB)

    Masi, G., E-mail: giulia.masi5@unibo.it [Dipartimento di Ingegneria Civile, Chimica, Ambientale e dei Materiali, Università di Bologna, via Terracini 28, 40131 Bologna (Italy); Chiavari, C., E-mail: cristina.chiavari@unibo.it [Dipartimento di Ingegneria Civile, Chimica, Ambientale e dei Materiali, Università di Bologna, via Terracini 28, 40131 Bologna (Italy); C.I.R.I. (Centro Interdipartimentale Ricerca Industriale) Meccanica Avanzata e Materiali, Università di Bologna, Bologna, via Terracini 28, 40131 Bologna (Italy); Avila, J., E-mail: jose.avila@synchrotron-soleil.fr [Synchrotron SOLEIL, L’Orme des Merisiers, 91190 Saint-Aubin (France); Esvan, J., E-mail: jerome.esvan@ensiacet.fr [Centre Interuniversitaire de Recherche et d’Ingénierie des Matériaux, Université de Toulouse, 4 allée Emile Monso, 31030 Toulouse (France); Raffo, S., E-mail: simona.raffo2@unibo.it [Dipartimento di Chimica Industriale “Toso Montanari”, Università di Bologna, viale Risorgimento 4, 40136 Bologna (Italy); Bignozzi, M.C., E-mail: maria.bignozzi@unibo.it [Dipartimento di Ingegneria Civile, Chimica, Ambientale e dei Materiali, Università di Bologna, via Terracini 28, 40131 Bologna (Italy); Asensio, M.C., E-mail: maria-carmen.asensio@synchrotron-soleil.fr [Synchrotron SOLEIL, L’Orme des Merisiers, 91190 Saint-Aubin (France); Robbiola, L., E-mail: robbiola@univ-tlse2.fr [TRACES Lab (CNRS UMR5608), Université Toulouse Jean-Jaurès, 5, allées Antonio-Machado, 31058 Toulouse (France); and others

    2016-03-15

    Graphical abstract: - Highlights: • Fire-gilded bronze prepared by ancient methods (Au–Hg layer on Cu–Sn–Zn–Pb–Sb). • Heating during gilding induces Sn and Znenrichment in the top part of the gilded layer. • SR-HRPES mapping of corrosion craters (cross-section) after accelerated ageing. • Selective dissolution of Cu and Zn in the craters induces Sn species enrichment. • The main species in the craters are related to hydroxi-oxide compounds. - Abstract: Gilded bronzes are often affected by severe corrosion, due to defects in the Au layer and Au/Cu alloy galvanic coupling, stimulated by large cathodic area of the gilded layer. Galvanic corrosion, triggered by gilding defects, leads to products growth at the Au/bronze interface, inducing blistering or break-up of the Au layer. In this context, fire-gilded bronze replicas prepared by ancient methods (use of spreadable Au–Hg paste) was specifically characterised by compiling complementary spectroscopic and imaging information before/after accelerated ageing with synthetic rain. Fire-gilded bronze samples were chemically imaged in cross-section at nano-metric scale (<200 nm) using high energy and lateral resolution synchrotron radiation photoemission (HR-SRPES) of core levels and valence band after conventional characterisation of the samples by Glow Discharge optical Emission Spectroscopy (GD-OES) and conventional X-ray photoelectron spectroscopy (XPS). We have found a net surface enrichment in Zn and Sn after fire-gilding and presence of metallic Hg, Pb and Cu within the Au layer. Moreover, the composition distribution of the elements together with their oxidation has been determined. It was also revealed that metallic phases including Hg and Pb remain in the gilding after corrosion. Moreover, selective dissolution of Zn and Cu occurs in the crater due to galvanic coupling, which locally induces relative Sn species enrichment (decuprification). The feasibility advantages and disadvantages of

  16. An almost knowledge-free approach to XPS intensity evaluation where use of atomic photoemission cross sections suffices for yielding material-specific inelastic background

    Energy Technology Data Exchange (ETDEWEB)

    Jo, Masatoshi, E-mail: m-jo@aist.go.jp

    2017-02-15

    Highlights: • Self-contained XPS background optimization based on the Tougaard’s formula. • Consistent core and Auger intensities for Cu metal. • Determination of intractable solid-state effects not required. • Realistic result restorable without using sample’s characteristic properties. • Estimation of IMFP from peak intensities and cross sections. - Abstract: A general procedure for peak intensity evaluation on the inelastic background of X-ray photoelectron spectra (XPS) has been developed, which is made up of tasks in three nested levels, level I, II and III. The task in level I is a simple background optimization for the case when the inelastic mean free path (IMFP, denoted λ(E)) and other constraints are given in advance [M. Jo, Surf. Interface Anal., 2003, 35, 729–737]. In order to find appropriate constraints, a batch job, which is a series of single jobs with systematically varied constraints, is constructed and iteratively solved in level II by improving the constraints from the viewpoint of how successfully the background is subtracted. It is found that, by the task in level II, for polycrystal Cu metal, the spectrum after inelastic background subtraction still contains a baseline component proportional to E{sup −k}, where E (>50 eV) is the electron kinetic energy and the exponent k around 2.4. This baseline is attributed to the high-energy tail of primary excitation spectrum of true secondary electron emission. The relative core intensities thus determined are in good agreement with the Scofield’s photoexcitation cross sections. The relation of core and Auger peak intensities is consistent as demonstrated by the fact that the sum of Cu 2p and 2s equals that of all Cu LMM peaks. The level III calculation is designed for the general case where λ is not available before the analysis. The relative energy dependence of λ except for the absolute value can be estimated by iterating the level II tasks with updated λ(E), based on the

  17. TOURE ALI.xps

    African Journals Online (AJOL)

    HP Pro 2000

    irrigated-rice production enterprise revealed positive economic profitability for both ... marketing in which a great number of women rice traders are active. ..... Table 3 : Summary results for single-factor change scenarios: increase in yield and ...

  18. KOKO KL.xps

    African Journals Online (AJOL)

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    En Côte d'Ivoire, le cacaoyer (Theobroma cacao L.) est traditionnellement cultivé selon un système extensif et itinérant, utilisant du matériel végétal peu performant. Les rendements en cacao sont donc faible (260 à 600 kg·ha-1·an-1). Pour améliorer la productivité des cacaoyères, les chercheurs ivoiriens ont mis au point.

  19. DJODJOUWIN 2.xps

    African Journals Online (AJOL)

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    guinéennes au Bénin. Terminalia superba est un arbre caractéristique des forêts denses semi-décidues, envahissant les recrûs secondaires. L'espèce est grégaire, de pleine lumière et à croissance rapide. Holoptelea grandis est une espèce exigeante.

  20. SOUMAHORO A..xps

    African Journals Online (AJOL)

    AISA

    avant le semis dans des boîtes de Pétri, sur du papier filtre ou sur le milieu de base de Murashige et Skoog. (MS). Sur le papier filtre, l'imbibition dans l'eau distillée des graines, pendant 24 heures, a donné le meilleur taux de germination (59,01 %). La stérilisation des graines dans l'acide sulfurique 96 % durant 1 minute,.

  1. BAMBA Vamoussa.xps

    African Journals Online (AJOL)

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    However, analysis showed a reduction of 12.31 % of work time with chemical maintenance and 21.04 % for mixed maintenance. Therefore, mixed maintenance practice appeared to be the major workforce that has to be mastered. Keywords : Rubber, maintenance costs, immature culture, a comparative study, Cote d'Ivoire.

  2. YABILE KR.xps

    African Journals Online (AJOL)

    HP Pro 2000

    favorable à la mise en œuvre d'une politique agricole visant la couverture des besoins alimentaires nationaux. ... surévaluation du taux de change du franc CFA ... Le taux de couverture national des besoins est de 44,6 % pour la viande et abats et de 12,6 % pour le lait et les produits laitiers. Au cours de ces dernières.

  3. Direct correlations between XPS analyses and growth film by chronopotentiometry on InP in liquid ammonia (−55 °C)

    Energy Technology Data Exchange (ETDEWEB)

    Gonçalves, A.-M., E-mail: anne-marie.goncalves@uvsq.fr; Njel, C.; Aureau, D.; Etcheberry, A.

    2017-01-01

    Highlights: • Anodic galvannostatic treatment on n‐InP is carried out in liquid ammonia (−55 °C) under illumination. • Whatever the anodic charge, a phosphazene like film is revealed by XPS without thickening of the layer. • The film growth requires a nucleation step which is followed by a phosphazene coalescence phenomenon in the two dimensions of the surface. • A monolayer film of phosphazene is suggested and an excess of charge is observed which can be assigned to ammonia oxidation. - Abstract: This paper is based on the understanding of the formation of a reproducible polyphosphazene-like film (−[(H{sub 2}N)−P=N]{sub n}−) obtained on InP by anodic treatment in liquid ammonia. The approach is innovative as it combines indications from the coulometric charges and the related chemical information from XPS analyses. Anodic charges are accurately monitored by galvanostatic treatment between 0.05 mC cm{sup −2} and 12.5 mC cm{sup −2}. XPS investigation of the treated surfaces demonstrates the presence of an anodic film on InP. Whatever the spent charge, the specific P{sub 2p} and N{sub 1s} signals agree with the growth of an ultrathin phosphazene layer. From 0.25 mC cm{sup −2} to 12.5 mC cm{sup −2}, a quasi constant XPS response is revealed without thickening of the film. However a gradual chemical evolution of the modified surface is clearly observed for the lower anodic charges (from 0.04 mC cm{sup −2} to 0.5 mC cm{sup −2}). In this case, the surface is entirely recovered by the film as soon as 0.25 mC cm{sup −2} is consumed at the interface. Same atomic surface ratios are indeed revealed indicating that a constant chemical composition is consistent with a polyphosphazene film. On the basis of atomic surface ratios evolutions determined by XPS, a mechanism of the film growth is deduced. It requires a nucleation step which is followed by a phosphazene coalescence phenomenon in the two dimensions of the surface. A final phosphazene

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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 Si 2+ and Al 2+ cation mobility under the influence of voltage potential between the cathode and anode will be discussed in detail

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

    Energy Technology Data Exchange (ETDEWEB)

    Embong, Zaidi, E-mail: zaidi@uthm.edu.my [Faculty of Science, Technology and Human Development, Universiti Tun Hussien Onn Malaysia (UTHM) 86400, Parit Raja, Batu, Johor (Malaysia); Research Centre for Soft Soils (RECESS), Office for Research, Innovation, Commercialization and Consultancy Management (ORICC), Universiti Tun Hussien Onn Malaysia UTHM 86400, Parit Raja, Batu, Johor (Malaysia); Johar, Saffuwan [Faculty of Science, Technology and Human Development, Universiti Tun Hussien Onn Malaysia (UTHM) 86400, Parit Raja, Batu, Johor (Malaysia); Tajudin, Saiful Azhar Ahmad [Research Centre for Soft Soils (RECESS), Office for Research, Innovation, Commercialization and Consultancy Management (ORICC), Universiti Tun Hussien Onn Malaysia UTHM 86400, Parit Raja, Batu, Johor (Malaysia); Sahdan, Mohd Zainizan [Microelectronics and Nanotechnology Centre (MiNT-SRC), Office for Research, Innovation, Commercialization and Consultancy Management (ORICC), Universiti Tun Hussien Onn Malaysia UTHM 86400, Parit Raja, Batu, Johor (Malaysia)

    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.

  6. Macroscopic and microscopic investigation of Ni(II) sequestration on diatomite by batch, XPS, and EXAFS techniques.

    Science.gov (United States)

    Sheng, Guodong; Yang, Shitong; Sheng, Jiang; Hu, Jun; Tan, Xiaoli; Wang, Xiangke

    2011-09-15

    Sequestration of Ni(II) on diatomite as a function of time, pH, and temperature was investigated by batch, XPS, and EXAFS techniques. The ionic strength-dependent sorption at pH < 7.0 was consistent with outer-sphere surface complexation, while the ionic strength-independent sorption at pH = 7.0-8.6 was indicative of inner-sphere surface complexation. EXAFS results indicated that the adsorbed Ni(II) consisted of ∼6 O at R(Ni-O) ≈ 2.05 Å. EXAFS analysis from the second shell suggested that three phenomena occurred at the diatomite/water interface: (1) outer-sphere and/or inner-sphere complexation; (2) dissolution of Si which is the rate limiting step during Ni uptake; and (3) extensive growth of surface (co)precipitates. Under acidic conditions, outer-sphere complexation is the main mechanism controlling Ni uptake, which is in good agreement with the macroscopic results. At contact time of 1 h or 1 day or pH = 7.0-8.0, surface coprecipitates occur concurrently with inner-sphere complexes on diatomite surface, whereas at contact time of 1 month or pH = 10.0, surface (co)precipitates dominate Ni uptake. Furthermore, surface loading increases with temperature increasing, and surface coprecipitates become the dominant mechanism at elevated temperature. The results are important to understand Ni interaction with minerals at the solid-water interface, which is helpful to evaluate the mobility of Ni(II) in the natural environment.

  7. Chemical state analysis of heat-treated 6, 13-bis(triisopropylsilylethynyl) pentacene investigated by XPS valence band spectra, XANES spectra and first-principles calculation

    International Nuclear Information System (INIS)

    Muro, Maiko; Natsume, Yutaka; Kikuma, Jun; Setoyama, Hiroyuki

    2014-01-01

    X-ray photoelectron spectroscopy (XPS) valence band spectra reflect the chemical bonding states. To take this advantage, we tried to interpret experimental spectra by the occupied density of states (DOS) based on first principles calculation. In this work, we discussed XPS and X-ray Absorption Near Edge Structure (XANES) spectra of 6, 13-bis(triisopropylsilylethynyl) pentacene (TIPS-Pen), which is well known as an organic semiconductor. We studied chemical structure change of TIPS-Pen caused by heat-treatment at 300degC under nitrogen and under the air. It has been suggested that the structural change of pentacene skeleton by Diels-Alder type reaction occurs in both cases. In addition, the sample heat-treated under the air showed desorption of the isopropyl group and increase of oxygen concentration. (author)

  8. Characterization of SiC in DLC/a-Si films prepared by pulsed filtered cathodic arc using Raman spectroscopy and XPS

    International Nuclear Information System (INIS)

    Srisang, C.; Asanithi, P.; Siangchaew, K.; Pokaipisit, A.; Limsuwan, P.

    2012-01-01

    DLC/a-Si films were deposited on germanium substrates. a-Si film was initially deposited as a seed layer on the substrate using DC magnetron sputtering. DLC film was then deposited on the a-Si layer via a pulsed filtered cathodic arc (PFCA) system. In situ ellipsometry was used to monitor the thicknesses of the growth films, allowing a precise control over the a-Si and DLC thicknesses of 6 and 9 nm, respectively. It was found that carbon atoms implanting on a-Si layer act not only as a carbon source for DLC formation, but also as a source for SiC formation. The Raman peak positions at 796 cm -1 and 972 cm -1 corresponded to the LO and TO phonon modes of SiC, respectively, were observed. The results were also confirmed using TEM, XPS binding energy and XPS depth profile analysis.

  9. XPS and ToF-SIMS analysis of natural rubies and sapphires heat-treated in a reducing (5 mol% H 2/Ar) atmosphere

    Science.gov (United States)

    Achiwawanich, S.; James, B. D.; Liesegang, J.

    2008-12-01

    Surface effects on Mong Hsu rubies and Kanchanaburi sapphires after heat treatment in a controlled reducing atmosphere (5 mol% H 2/Ar) have been investigated using advanced surface science techniques including X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Visual appearance of the gemstones is clearly affected by the heat treatment in a reducing atmosphere. Kanchanaburi sapphires, in particular, exhibit Fe-containing precipitates after the heat treatment which have not been observed in previous studies under an inert atmosphere. Significant correlation between changes in visual appearance of the gemstones and variations in surface concentration of trace elements, especially Ti and Fe are observed. The XPS and ToF-SIMS results suggest that; (1) a reducing atmosphere affects the oxidation state of Fe; (2) dissociation of Fe-Ti interaction may occur during heat treatment.

  10. XPS and ToF-SIMS analysis of natural rubies and sapphires heat-treated in a reducing (5 mol% H{sub 2}/Ar) atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Achiwawanich, S. [Department of Physics, La Trobe University, VIC 3086 (Australia); Centre for Materials and Surface Science, La Trobe University, VIC 3086 (Australia); James, B.D. [Centre for Materials and Surface Science, La Trobe University, VIC 3086 (Australia); Department of Chemistry, La Trobe University, VIC 3086 (Australia); Liesegang, J. [Department of Physics, La Trobe University, VIC 3086 (Australia); Centre for Materials and Surface Science, La Trobe University, VIC 3086 (Australia)], E-mail: J.Liesegang@latrobe.edu.au

    2008-12-30

    Surface effects on Mong Hsu rubies and Kanchanaburi sapphires after heat treatment in a controlled reducing atmosphere (5 mol% H{sub 2}/Ar) have been investigated using advanced surface science techniques including X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Visual appearance of the gemstones is clearly affected by the heat treatment in a reducing atmosphere. Kanchanaburi sapphires, in particular, exhibit Fe-containing precipitates after the heat treatment which have not been observed in previous studies under an inert atmosphere. Significant correlation between changes in visual appearance of the gemstones and variations in surface concentration of trace elements, especially Ti and Fe are observed. The XPS and ToF-SIMS results suggest that; (1) a reducing atmosphere affects the oxidation state of Fe; (2) dissociation of Fe-Ti interaction may occur during heat treatment.

  11. Surface analysis of glass fibres using XPS and AFM: case study of glass fibres recovered from the glass fibre reinforced polymer using chemical recycling

    Science.gov (United States)

    Nzioka, A. M.; Kim, Y. J.

    2018-01-01

    In this study, we present the results of an experimental study of the use of the X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) to characterise the coatings of the recovered E - glass fibres. The recovered E - glass fibres were obtained using chemical recycling process coupled with ultrasound cavitation. The objective of this study was to analyse the impact of chemical recycling and the ultrasound cavitation process on the sizing properties of the recovered fibres. We obtained the recovered fibres and sized using 1 wt% 3 - aminopropyltriethoxysilane (APS). Part of the sized fibres was washed with acetone and analysed all the sample fibres using AFM and XPS. Results showed the different composition of sizing after extraction using acetone. We compared the results of this study with that of virgin clean glass fibres.

  12. Determination of trace metals in TSP and PM2.5 materials collected in the Metropolitan Area of Monterrey, Mexico: A characterization study by XPS, ICP-AES and SEM-EDS

    Science.gov (United States)

    González, Lucy T.; Longoria Rodríguez, F. E.; Sánchez-Domínguez, M.; Cavazos, Aleyda; Leyva-Porras, C.; Silva-Vidaurri, L. G.; Askar, Karim Acuña; Kharissov, B. I.; Villarreal Chiu, J. F.; Alfaro Barbosa, J. M.

    2017-11-01

    The concentration levels of trace metals of toxicological importance were evaluated in the total suspended particles (TSP) and particulate matter smaller than 2.5 μm (PM2.5) collected in the Metropolitan Area of Monterrey (MAM) in Mexico. Samples were characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy with an energy-dispersive spectroscopy system (SEM-EDS). In addition, the data were statistically treated by the methodology of Pearson Correlation (PC) and Principal Components Analysis (PCA) to identify the possible emitting sources. Surface analysis of the particulate matter (PM) by XPS revealed that the most abundant elements were Ca, Al, Na, Zn, Cu and Mg. The deconvolution of the Ca2p, Zn2p and Cu2p signals showed that the main contributors were CaCO3, ZnO and Cu/Cu2O, respectively. The bulk analysis of the PM by ICP-AES showed Fe, Cu and Zn as the most abundant elements. Fe-rich particles presented two different morphologies: the prismatic particles were associated with a natural origin, while the spherical particles with anthropogenic sources. The Zn and Cu were predominantly observed in the sampling stations with high vehicular traffic, and the emitting sources were associated with the burning of fuels from automobiles and the wear of the tires and brakes. The highest concentration of Pb was detected in the sampling station located near the industrial zones, and its cause was associated with the ceramic and glass industries, the burning of fuel oil in power plants and the production of lead-based batteries for automobiles.

  13. XPS-nanocharacterization of organic layers electrochemically grafted on the surface of SnO_2 thin films to produce a new hybrid material coating

    International Nuclear Information System (INIS)

    Drevet, R.; Dragoé, D.; Barthés-Labrousse, M.G.; Chaussé, A.; Andrieux, M.

    2016-01-01

    Graphical abstract: An innovative hybrid material layer is synthesized by combining two processes. SnO_2 thin films are deposited by MOCVD on Si substrates and an organic layer made of carboxyphenyl moieties is electrochemically grafted by the reduction of a diazonium salt. XPS characterizations are carried out to assess the efficiency of the electrochemical grafting. Display Omitted - Highlights: • An innovative hybrid material layer is synthesized by combining two processes. • SnO_2 thin films are deposited by MOCVD on Si substrates. • An organic layer is electrochemically grafted by the reduction of a diazonium salt. • The efficiency of the grafting is accurately assessed by XPS. • Three electrochemical grafting models are proposed. - Abstract: This work presents the synthesis and the characterization of hybrid material thin films obtained by the combination of two processes. The electrochemical grafting of organic layers made of carboxyphenyl moieties is carried out from the reduction of a diazonium salt on tin dioxide (SnO_2) thin films previously deposited on Si substrates by metal organic chemical vapor deposition (MOCVD). Since the MOCVD experimental parameters impact the crystal growth of the SnO_2 layer (i.e. its morphology and its texturation), various electrochemical grafting models can occur, producing different hybrid materials. In order to evidence the efficiency of the electrochemical grafting of the carboxyphenyl moieties, X-ray Photoelectron Spectroscopy (XPS) is used to characterize the first nanometers in depth of the synthesized hybrid material layer. Then three electrochemical grafting models are proposed.

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  15. Electronic state of ruthenium deposited onto oxide supports: An XPS study taking into account the final state effects

    International Nuclear Information System (INIS)

    Larichev, Yurii V.; Moroz, Boris L.; Bukhtiyarov, Valerii I.

    2011-01-01

    The electronic state of ruthenium in the supported Ru/EO x (EO x = MgO, Al 2 O 3 or SiO 2 ) catalysts prepared by with the use of Ru(OH)Cl 3 or Ru(acac) 3 (acac = acetylacetonate) and reduced with H 2 at 723 K is characterized by X-ray photoelectron spectroscopy (XPS) in the Ru 3d, Cl 2p and O 1s regions. The influence of the final state effects (the differential charging and variation of the relaxation energy) on the binding energy (BE) of Ru 3d 5/2 core level measured for supported Ru nanoparticles is estimated by comparison of the Fermi levels and the modified Auger parameters determined for the Ru/EO x samples with the corresponding characteristics of the bulk Ru metal. It is found that the negative shift of the Ru 3d 5/2 peak which is observed in the spectrum of ruthenium deposited onto MgO (BE = 279.5-279.7 eV) with respect to that of Ru black (BE = 280.2 eV) or ruthenium supported on γ-Al 2 O 3 and SiO 2 (BE = 280.4 eV) is caused not by the transfer of electron density from basic sites of MgO, as considered earlier, but by the differential charging of the supported Ru particles compared with the support surface. Correction for the differential charging value reveals that the initial state energies of ruthenium in the Ru/EO x systems are almost identical (BE = 280.5 ± 0.1 eV) irrespectively of acid-base properties of the support, the mean size of supported Ru crystallites (within the range of 2-10 nm) and the surface Cl content. The results obtained suggest that the difference in ammonia synthesis activity between the Ru catalysts supported on MgO and on the acidic supports is accounted for by not different electronic state of ruthenium on the surface of these oxides but by some other reasons.

  16. Wettability and XPS analyses of nickel–phosphorus surfaces after plasma treatment: An efficient approach for surface qualification in mechatronic processes

    International Nuclear Information System (INIS)

    Vivet, L.; Joudrier, A.-L.; Bouttemy, M.; Vigneron, J.; Tan, K.L.; Morelle, J.M.; Etcheberry, A.; Chalumeau, L.

    2013-01-01

    Electroless nickel-high-phosphorus Ni–P plating is known for its physical properties. In case of electronic and mechatronic assembly processes achieved under ambient conditions the wettability of the Ni–P layer under ambient temperature and ambient air stays a point of surface quality investigation. This contribution will be devoted to the study of the surface properties of Ni–P films for which we performed air plasma treatment. We focus our attention on the evolution of the surface wettability, using the classical sessile drop technique. Interpreting the results with the OWRK model we extract the polar and disperse surface tension components from which we deduced typical evolution of the surface properties with the different treatment settings. By controlling the variations of the parameters of the plasma exposure we are able to change the responses of our Ni–P sample from total hydrophobic to total hydrophilic behaviours. All the intermediate states can be reached by adapting the treatment parameters. So it is demonstrated that the apparent Ni–P surface properties can be fully adapted and the surface setting can be well characterized by wettability measurements. To deep our knowledge of the surface modifications induced by plasma we performed parallel SEM and XPS analyses which provide informations on the structure and the chemical composition of the surface for each set of treatment parameters. Using this double approach we were able to propose a correlation between the evolution of surface chemical composition and surface wettability which are completely governed by the plasma treatment conditions. Chemical parameters as the elimination of the carbon contamination, the progressive surface oxidation, and the slight incorporation of nitrogen due to the air plasma interaction are well associated with the evolution of the wettability properties. So a complete engineering for the Ni–P surface preparation has been established. The sessile drop method can

  17. Wettability and XPS analyses of nickel-phosphorus surfaces after plasma treatment: An efficient approach for surface qualification in mechatronic processes

    Science.gov (United States)

    Vivet, L.; Joudrier, A.-L.; Bouttemy, M.; Vigneron, J.; Tan, K. L.; Morelle, J. M.; Etcheberry, A.; Chalumeau, L.

    2013-06-01

    Electroless nickel-high-phosphorus Ni-P plating is known for its physical properties. In case of electronic and mechatronic assembly processes achieved under ambient conditions the wettability of the Ni-P layer under ambient temperature and ambient air stays a point of surface quality investigation. This contribution will be devoted to the study of the surface properties of Ni-P films for which we performed air plasma treatment. We focus our attention on the evolution of the surface wettability, using the classical sessile drop technique. Interpreting the results with the OWRK model we extract the polar and disperse surface tension components from which we deduced typical evolution of the surface properties with the different treatment settings. By controlling the variations of the parameters of the plasma exposure we are able to change the responses of our Ni-P sample from total hydrophobic to total hydrophilic behaviours. All the intermediate states can be reached by adapting the treatment parameters. So it is demonstrated that the apparent Ni-P surface properties can be fully adapted and the surface setting can be well characterized by wettability measurements. To deep our knowledge of the surface modifications induced by plasma we performed parallel SEM and XPS analyses which provide informations on the structure and the chemical composition of the surface for each set of treatment parameters. Using this double approach we were able to propose a correlation between the evolution of surface chemical composition and surface wettability which are completely governed by the plasma treatment conditions. Chemical parameters as the elimination of the carbon contamination, the progressive surface oxidation, and the slight incorporation of nitrogen due to the air plasma interaction are well associated with the evolution of the wettability properties. So a complete engineering for the Ni-P surface preparation has been established. The sessile drop method can be

  18. High resolution SAW elastography for ex-vivo porcine skin specimen

    Science.gov (United States)

    Zhou, Kanheng; Feng, Kairui; Wang, Mingkai; Jamera, Tanatswa; Li, Chunhui; Huang, Zhihong

    2018-02-01

    Surface acoustic wave (SAW) elastography has been proven to be a non-invasive, non-destructive method for accurately characterizing tissue elastic properties. Current SAW elastography technique tracks generated surface acoustic wave impulse point by point which are a few millimeters away. Thus, reconstructed elastography has low lateral resolution. To improve the lateral resolution of current SAW elastography, a new method was proposed in this research. A M-B scan mode, high spatial resolution phase sensitive optical coherence tomography (PhS-OCT) system was employed to track the ultrasonically induced SAW impulse. Ex-vivo porcine skin specimen was tested using this proposed method. A 2D fast Fourier transform based algorithm was applied to process the acquired data for estimating the surface acoustic wave dispersion curve and its corresponding penetration depth. Then, the ex-vivo porcine skin elastogram was established by relating the surface acoustic wave dispersion curve and its corresponding penetration depth. The result from the proposed method shows higher lateral resolution than that from current SAW elastography technique, and the approximated skin elastogram could also distinguish the different layers in the skin specimen, i.e. epidermis, dermis and fat layer. This proposed SAW elastography technique may have a large potential to be widely applied in clinical use for skin disease diagnosis and treatment monitoring.

  19. XPS, UV–vis spectroscopy and AFM studies on removal mechanisms of Si-face SiC wafer chemical mechanical polishing (CMP)

    International Nuclear Information System (INIS)

    Zhou, Yan; Pan, Guoshun; Shi, Xiaolei; Xu, Li; Zou, Chunli; Gong, Hua; Luo, Guihai

    2014-01-01

    Highlights: • CMP removal mechanism of Si-face SiC wafer is investigated through XPS analysis. • UV–vis spectroscopy is used to study CMP removal mechanisms. • CMP removal model of Si-face SiC wafer is proposed. • The variations of atomic step morphology on ultra-smooth surface via AFM is studied. - Abstract: Chemical mechanical polishing (CMP) removal mechanisms of on-axis Si-face SiC wafer have been investigated through X-ray photoelectron spectroscopy (XPS), UV–visible (UV–vis) spectroscopy and atomic force microscopy (AFM). XPS results indicate that silicon oxide is formed on Si-face surface polished by the slurry including oxidant H 2 O 2 , but not that after immersing in H 2 O 2 solution. UV–vis spectroscopy curves prove that • OH hydroxyl radical could be generated only under CMP polishing by the slurry including H 2 O 2 and abrasive, so as to promote oxidation of Si-face to realize the effective removal; meanwhile, alkali KOH during CMP could induce the production of more radicals to improve the removal. On the other side, ultra-smooth polished surface with atomic step structure morphology and extremely low Ra of about 0.06 nm (through AFM) is obtained using the developed slurry with silica nanoparticle abrasive. Through investigating the variations of the atomic step morphology on the surface polished by different slurries, it's reveals that CMP removal mechanism involves a simultaneous process of surface chemical reaction and nanoparticle atomic scale abrasion

  20. In situ NAP-XPS spectroscopy during methane dry reforming on ZrO2/Pt(1 1 1) inverse model catalyst

    Science.gov (United States)

    Rameshan, C.; Li, H.; Anic, K.; Roiaz, M.; Pramhaas, V.; Rameshan, R.; Blume, R.; Hävecker, M.; Knudsen, J.; Knop-Gericke, A.; Rupprechter, G.

    2018-07-01

    Due to the need of sustainable energy sources, methane dry reforming is a useful reaction for conversion of the greenhouse gases CH4 and CO2 to synthesis gas (CO  +  H2). Syngas is the basis for a wide range of commodity chemicals and can be utilized for fuel production via Fischer–Tropsch synthesis. The current study focuses on spectroscopic investigations of the surface and reaction properties of a ZrO2/Pt inverse model catalyst, i.e. ZrO2 particles (islands) grown on a Pt(1 1 1) single crystal, with emphasis on in situ near ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) during MDR reaction. In comparison to technological systems, model catalysts facilitate characterization of the surface (oxidation) state, surface adsorbates, and the role of the metal-support interface. Using XPS and infrared reflection absorption spectroscopy we demonstrated that under reducing conditions (UHV or CH4) the ZrO2 particles transformed to an ultrathin ZrO2 film that started to cover (wet) the Pt surface in an SMSI-like fashion, paralleled by a decrease in surface/interface oxygen. In contrast, (more oxidizing) dry reforming conditions with a 1:1 ratio of CH4 and CO2 were stabilizing the ZrO2 particles on the model catalyst surface (or were even reversing the strong metal support interaction (SMSI) effect), as revealed by in situ XPS. Carbon deposits resulting from CH4 dissociation were easily removed by CO2 or by switching to dry reforming conditions (673–873 K). Thus, at these temperatures the active Pt surface remained free of carbon deposits, also preserving the ZrO2/Pt interface.

  1. XPS-nanocharacterization of organic layers electrochemically grafted on the surface of SnO{sub 2} thin films to produce a new hybrid material coating

    Energy Technology Data Exchange (ETDEWEB)

    Drevet, R., E-mail: richarddrevet@yahoo.fr [Univ. Paris Sud, SP2M-ICMMO, CNRS UMR 8182, Bât. 410, 91405 Orsay Cedex (France); Université d’Evry Val d’Essonne, LAMBE, CNRS-CEA UMR 8587, Boulevard François Mitterrand, 91025 Evry Cedex (France); Dragoé, D.; Barthés-Labrousse, M.G. [Univ. Paris Sud, SP2M-ICMMO, CNRS UMR 8182, Bât. 410, 91405 Orsay Cedex (France); Chaussé, A. [Université d’Evry Val d’Essonne, LAMBE, CNRS-CEA UMR 8587, Boulevard François Mitterrand, 91025 Evry Cedex (France); Andrieux, M. [Univ. Paris Sud, SP2M-ICMMO, CNRS UMR 8182, Bât. 410, 91405 Orsay Cedex (France)

    2016-10-30

    Graphical abstract: An innovative hybrid material layer is synthesized by combining two processes. SnO{sub 2} thin films are deposited by MOCVD on Si substrates and an organic layer made of carboxyphenyl moieties is electrochemically grafted by the reduction of a diazonium salt. XPS characterizations are carried out to assess the efficiency of the electrochemical grafting. Display Omitted - Highlights: • An innovative hybrid material layer is synthesized by combining two processes. • SnO{sub 2} thin films are deposited by MOCVD on Si substrates. • An organic layer is electrochemically grafted by the reduction of a diazonium salt. • The efficiency of the grafting is accurately assessed by XPS. • Three electrochemical grafting models are proposed. - Abstract: This work presents the synthesis and the characterization of hybrid material thin films obtained by the combination of two processes. The electrochemical grafting of organic layers made of carboxyphenyl moieties is carried out from the reduction of a diazonium salt on tin dioxide (SnO{sub 2}) thin films previously deposited on Si substrates by metal organic chemical vapor deposition (MOCVD). Since the MOCVD experimental parameters impact the crystal growth of the SnO{sub 2} layer (i.e. its morphology and its texturation), various electrochemical grafting models can occur, producing different hybrid materials. In order to evidence the efficiency of the electrochemical grafting of the carboxyphenyl moieties, X-ray Photoelectron Spectroscopy (XPS) is used to characterize the first nanometers in depth of the synthesized hybrid material layer. Then three electrochemical grafting models are proposed.

  2. Surface state modulation through wet chemical treatment as a route to controlling the electrical properties of ZnO nanowire arrays investigated with XPS

    International Nuclear Information System (INIS)

    Lord, Alex M.; Maffeis, Thierry G.; Allen, Martin W.; Morgan, David; Davies, Philip R.; Jones, Daniel R.; Evans, Jonathan E.; Smith, Nathan A.; Wilks, Steve P.

    2014-01-01

    Highlights: • Direct measurement of the surface band bending exhibited by ZnO nanowires using monochromatic XPS. • Modulation of the surface depletion region using wet chemical treatment (EtOH, H 2 O 2 ). • The measured surface potential barrier agrees with electrical measurements of individual nanowires. • H 2 O 2 depletes the nanowire of charge carriers while EtOH donates electrons at the surface. • EtOH has the effect of restoring the surface potential barrier of oxidised nanowires. - Abstract: ZnO is a wide bandgap semiconductor that has many potential applications including solar cell electrodes, transparent thin film transistors and gas/biological sensors. Since the surfaces of ZnO materials have no amorphous or oxidised layers, they are very environmentally sensitive, making control of their semiconductor properties challenging. In particular, the electronic properties of ZnO nanostructures are dominated by surface effects while surface conduction layers have been observed in thin films and bulk crystals. Therefore, the ability to use the ZnO materials in a controlled way depends on the development of simple techniques to modulate their surface electronic properties. Here, we use monochromatic x-ray photoelectron spectroscopy (XPS) to investigate the use of different wet chemical treatments (EtOH, H 2 O 2 ) to control the electronic properties of ZnO nanowires by modulating the surface depletion region. The valence band and core level XPS spectra are used to explore the relationship between the surface chemistry of the nanowires and the surface band bending

  3. Evaluation of process influences on surface chemistry of epoxy acrylate based solder mask via XPS, ToF-SIMS and contact angle measurement

    Energy Technology Data Exchange (ETDEWEB)

    Hofmeister, Caroline, E-mail: caroline.hofmeister@de.bosch.com [Robert Bosch GmbH, Postfach 30 02 40, 70442 Stuttgart (Germany); Fraunhofer Institute for Manufacturing Technology and Advanced Materials IFAM, Wiener Str. 12, 28359 Bremen (Germany); Maaß, Sebastian [Robert Bosch GmbH, Postfach 30 02 40, 70442 Stuttgart (Germany); Fladung, Thorsten; Mayer, Bernd [Fraunhofer Institute for Manufacturing Technology and Advanced Materials IFAM, Wiener Str. 12, 28359 Bremen (Germany)

    2017-01-01

    Epoxy acrylate based solder mask formulations were conditioned by different printed circuit board (PCB) manufacturing and PCB assembly process stages. Depending on these different influences the chemistry of the solder mask surface was investigated regarding adhesion to possible adhesion partners. The combination of X-ray photoelectron spectrometry (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and the contact angle method, for surface energy determination, provided a detailed understanding of the surface near region up to the topmost monolayer, which forms the contact zone in which adhesion takes place. The combination of ToF-SIMS and XPS provided molecular information of surface components comprising quantitative information. The influences of all process steps, like UV, chemical and thermal treatment, on the chemical surface composition and appearance were identified. Based on the results a chemical surface model could be created regarding the different adhesion mechanisms. It has been shown that an enrichment of siloxanes at the surface is generated by different mechanisms that were distinguished based on ToF-SIMS. Even though an oxidation process in the surface near region (10 nm) was indicated by XPS, no increase of the surface polar groups and thus no polarity increase could be observed within the first monolayer. A surface model derived from the analysis results shows generation and occupation of free sites at the surface through all stages of the process. An occupation of free sites by siloxanes from additives in the solder mask formulation results in a siloxane dominated topmost monolayer. - Highlights: • A surface model describing the process influences is proposed. • Detailed siloxane reaction analysis was possible with ToF-SIMS. • Photo-chemical, chemical and thermal surface modification occur during PCB manufacturing.

  4. Microstructure and electrical properties of slug-type resistors based on B4C and TiC - ESCA - XPS and impedance spectroscopy investigations

    International Nuclear Information System (INIS)

    Klimiec, E.; Zaraska, W.; Stobiecki, T.; Bak, W.; Starzyk, F.

    2000-01-01

    The microstructure and electrical properties of slug-type resistors based on B 4 C and TiC were investigated. From XPS measurements was deducted that Ti in TiO 2 is in intermediate oxidation number between Ti +4 and Ti +3 . The impedance of both type of resistors is independent on frequency in the range from 10 3 to 10 4 Hz, only very subtle differences above 10 4 Hz are observed. The metallic type conductivity in TiC and semiconducting in B 4 C was established. (author)

  5. Utilization of the statistics techniques for the analysis of the XPS (X-ray photoelectron spectroscopy) and Auger electronic spectra's deconvolutions

    International Nuclear Information System (INIS)

    Puentes, M.B.

    1987-01-01

    For the analysis of the XPS (X-ray photoelectron spectroscopy) and Auger spectra, it is important to performe the peaks' separation and estimate its intensity. For this purpose, a methodology was implemented, including: a spectrum's filter; b) substraction of the base line (or inelastic background); c) deconvolution (separation of the distribution that integrates the spectrum) and d) error of calculation of the mean estimation, comprising adjustment quality tests. A software (FORTRAN IV plus) that permits to use the methodology proposed from the experimental spectra was implemented. The quality of the methodology was tested with simulated spectra. (Author) [es

  6. Quantification of the toxic hexavalent chromium content in an organic matrix by X-ray photoelectron spectroscopy (XPS) and ultra-low-angle microtomy (ULAM)

    Science.gov (United States)

    Greunz, Theresia; Duchaczek, Hubert; Sagl, Raffaela; Duchoslav, Jiri; Steinberger, Roland; Strauß, Bernhard; Stifter, David

    2017-02-01

    Cr(VI) is known for its corrosion inhibitive properties and is, despite legal regulations, still a potential candidate to be added to thin (1-3 μm) protective coatings applied on, e.g., electrical steel as used for transformers, etc. However, Cr(VI) is harmful to the environment and to the human health. Hence, a reliable quantification of it is of decisive interest. Commonly, an alkaline extraction with a photometric endpoint detection of Cr(VI) is used for such material systems. However, this procedure requires an accurate knowledge on sample parameters such as dry film thickness and coating density that are occasionally associated with significant experimental errors. We present a comprehensive study of a coating system with a defined Cr(VI) pigment concentration applied on electrical steel. X-ray photoelectron spectroscopy (XPS) was employed to resolve the elemental chromium concentration and the chemical state. Turning to the fact that XPS is extremely surface sensitive (distribution inside the coating.

  7. Quantitative analysis of Ni2+/Ni3+ in Li[NixMnyCoz]O2 cathode materials: Non-linear least-squares fitting of XPS spectra

    Science.gov (United States)

    Fu, Zewei; Hu, Juntao; Hu, Wenlong; Yang, Shiyu; Luo, Yunfeng

    2018-05-01

    Quantitative analysis of Ni2+/Ni3+ using X-ray photoelectron spectroscopy (XPS) is important for evaluating the crystal structure and electrochemical performance of Lithium-nickel-cobalt-manganese oxide (Li[NixMnyCoz]O2, NMC). However, quantitative analysis based on Gaussian/Lorentzian (G/L) peak fitting suffers from the challenges of reproducibility and effectiveness. In this study, the Ni2+ and Ni3+ standard samples and a series of NMC samples with different Ni doping levels were synthesized. The Ni2+/Ni3+ ratios in NMC were quantitatively analyzed by non-linear least-squares fitting (NLLSF). Two Ni 2p overall spectra of synthesized Li [Ni0.33Mn0.33Co0.33]O2(NMC111) and bulk LiNiO2 were used as the Ni2+ and Ni3+ reference standards. Compared to G/L peak fitting, the fitting parameters required no adjustment, meaning that the spectral fitting process was free from operator dependence and the reproducibility was improved. Comparison of residual standard deviation (STD) showed that the fitting quality of NLLSF was superior to that of G/L peaks fitting. Overall, these findings confirmed the reproducibility and effectiveness of the NLLSF method in XPS quantitative analysis of Ni2+/Ni3+ ratio in Li[NixMnyCoz]O2 cathode materials.

  8. Microstructural study by XPS and GISAXS of surface layers formed via phase separation and percolation in polystyren/tetrabutyl titanate/alumina composite films

    International Nuclear Information System (INIS)

    Zeng Yanwei; Tian Changan; Liu Junliang

    2006-01-01

    The XPS and GISAXS have been employed as useful tools to probe the chemical compositional and microstructural evolutions in the surface layers formed via phase separation and percolation in polystyren/Ti(OBut) 4 /alumina composite thick films. The surface enrichment of Ti species due to the migration of Ti(OBut) 4 molecules in the films was found to show an incubation period of ∼15 h while the samples were treated at 100 deg. C before a remarkable progress can be identified. According to the XPS and GISAXS data, Key mechanism to govern this surface process is phenomenologically considered to be the specific phase separation behavior in Ti(OBut) 4 /PS blend and the subsequent percolating process. The extended thermal treatment was found to make the surface layer microstructure evolve from local phase separation featured with an increasing population of individual microbeads of Ti(OBut) 4 (∼1.5 nm in radius) to the formation of large size clusters of microbeads due to their interconnections, accompanied by the growth of every microbead itself to ∼10 nm on the average, which provokes and then enhances the surface enrichment of Ti(OBut) 4 since these clusters act as a fast diffusion network due to percolation effect

  9. Core-level XPS studies of Ce and La intermetallic compounds and their implications for the 4f levels of Ce compounds

    International Nuclear Information System (INIS)

    Freiburg, C.; Fuggle, J.C.; Hillebrecht, F.U.; Zolnierek, Z.; Laesser, R.

    1983-01-01

    The 3d core hole X-ray photoelectron spectra (XPS) of approximately 30 intermetallic compounds of La and Ce are reported. Transitions to final states with approximately f 0 , f 1 and f 2 character are observed in some Ce compounds (f 0 and f 1 for La compounds). The results are discussed in terms of the current ideas of the influence of f-counts and f-levels hybridization on core level lineshapes. We cannot find an explanatoin of the observed spectra consisted with the ''promotial model'' where the 4f-count varies and 4f electron was thought to be entirely promoted to the Ce 5d6s valence bands in some compounds. There may be some small charge transfer from the f level, however. In conjunction with ideas on screening processes in XPS the observed lineshapes suggest coupling of the 4f electrons to other states is strongest in those compounds previously thought to have f 0 character. This coupling increases despite a large increase in the Ce-Ce distance when Ce is diluted with Ni or Pd. Thus it cannot be due to direct f-f interaction and must be attributed to coupling with the other valence electrons; possibly those centred on the partner sites. (orig./EZ) [de

  10. XPS and STEM study of the interface formation between ultra-thin Ru and Ir OER catalyst layers and perylene red support whiskers

    Directory of Open Access Journals (Sweden)

    Atanasoska Ljiljana L.

    2013-01-01

    Full Text Available The interface formation between nano-structured perylene red (PR whiskers and oxygen evolution reaction (OER catalysts ruthenium and iridium has been studied systematically by XPS and STEM. The OER catalyst over-layers with thicknesses ranging from ~0.1 to ~50 nm were vapor deposited onto PR ex-situ. STEM images demonstrate that, with increasing thickness, Ru and Ir transform from amorphous clusters to crystalline nanoparticles, which agglomerate with increased over-layer thickness. XPS data show a strong interaction between Ru and PR. Ir also interacts with PR although not to the extent seen for Ru. At low coverages, the entire Ru deposit is in the reacted state while a small portion of the deposited Ir remains metallic. Ru and Ir bonding occur at the PR carbonyl sites as evidenced by the attenuation of carbonyl photoemission and the emergence of new peak assigned to C-O single bond. The curve fitting analysis and the derived stoichiometry indicates the formation of metallo-organic bonds. The co-existence of oxide bonds is also apparent.

  11. Initial stages of high temperature metal oxidation

    International Nuclear Information System (INIS)

    Yang, C.Y.; O'Grady, W.E.

    1981-01-01

    The application of XPS and UPS to the study of the initial stages of high temperature (> 350 0 C) electrochemical oxidation of iron and nickel is discussed. In the high temperature experiments, iron and nickel electrodes were electrochemically oxidized in contact with a solid oxide electrolyte in the uhv system. The great advantages of this technique are that the oxygen activity at the interface may be precisely controlled and the ability to run the reactions in uhv allows the simultaneous observation of the reactions by XPS

  12. Synergism between rare earth cerium(IV) ion and vanillin on the corrosion of steel in H{sub 2}SO{sub 4} solution: Weight loss, electrochemical, UV-vis, FTIR, XPS, and AFM approaches

    Energy Technology Data Exchange (ETDEWEB)

    Li Xianghong [Department of Fundamental Courses, Southwest Forestry University, Kunming 650224 (China)], E-mail: xianghong-li@163.com; Deng Shuduan [Department of Wood Science and Technology, Southwest Forestry University, Kunming 650224 (China); Fu Hui [Department of Fundamental Courses, Southwest Forestry University, Kunming 650224 (China); Mu Guannan [Department of Chemistry, Yunnan University, Kunming 650091 (China); Zhao Ning [Department of Fundamental Courses, Southwest Forestry University, Kunming 650224 (China)

    2008-06-30

    The synergism between rare earth cerium(IV) ion and vanillin (4-hydroxy-3-methoxy-benzaldehyde) on the corrosion of cold rolled steel (CRS) in 1.0 M H{sub 2}SO{sub 4} solution at five temperatures ranging from 20 to 60 deg. C was first studied by weight loss and potentiodynamic polarization methods. The inhibited solutions were analyzed by ultraviolet and visible spectrophotometer (UV-vis). The adsorbed film of CRS surface containing optimum doses of the blends Ce{sup 4+}-vanillin was investigated by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and atomic force microscope (AFM). The results revealed that vanillin had a moderate inhibitive effect, and the inhibition efficiency (IE) increased with the vanillin concentration. The adsorption of vanillin obeyed Temkin adsorption isotherm. Polarization curves showed that vanillin was a mixed-type inhibitor in sulfuric acid, while prominently inhibited the cathodic reaction. For the cerium(IV) ion, it had a negligible effect, and the maximum IE was only about 20%. However, incorporation of Ce{sup 4+} with vanillin improved significantly the inhibition performance. The IE for Ce{sup 4+} in combination with vanillin was higher than the summation of IE for single Ce{sup 4+} and single vanillin, which was synergism in nature. A high inhibition efficiency, 98% was obtained by a mixture of 25-200 mg l{sup -1} vanillin and 300-475 mg l{sup -1} Ce{sup 4+}. UV-vis showed that the new complex of Ce{sup 4+}-vanillin was formed in 1.0 M H{sub 2}SO{sub 4} for Ce{sup 4+} combination with vanillin. Polarization studies showed that the complex of Ce{sup 4+}-vanillin acted as a mixed-type inhibitor, which drastically inhibits both anodic and cathodic reactions. FTIR and XPS revealed that a protective film formed in the presence of both vanillin and Ce{sup 4+} was composed of cerium oxide and the complex of Ce{sup 4+}-vanillin. The synergism between Ce{sup 4+} and vanillin could also be evidenced

  13. Synergism between rare earth cerium(IV) ion and vanillin on the corrosion of steel in H2SO4 solution: Weight loss, electrochemical, UV-vis, FTIR, XPS, and AFM approaches

    International Nuclear Information System (INIS)

    Li Xianghong; Deng Shuduan; Fu Hui; Mu Guannan; Zhao Ning

    2008-01-01

    The synergism between rare earth cerium(IV) ion and vanillin (4-hydroxy-3-methoxy-benzaldehyde) on the corrosion of cold rolled steel (CRS) in 1.0 M H 2 SO 4 solution at five temperatures ranging from 20 to 60 deg. C was first studied by weight loss and potentiodynamic polarization methods. The inhibited solutions were analyzed by ultraviolet and visible spectrophotometer (UV-vis). The adsorbed film of CRS surface containing optimum doses of the blends Ce 4+ -vanillin was investigated by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and atomic force microscope (AFM). The results revealed that vanillin had a moderate inhibitive effect, and the inhibition efficiency (IE) increased with the vanillin concentration. The adsorption of vanillin obeyed Temkin adsorption isotherm. Polarization curves showed that vanillin was a mixed-type inhibitor in sulfuric acid, while prominently inhibited the cathodic reaction. For the cerium(IV) ion, it had a negligible effect, and the maximum IE was only about 20%. However, incorporation of Ce 4+ with vanillin improved significantly the inhibition performance. The IE for Ce 4+ in combination with vanillin was higher than the summation of IE for single Ce 4+ and single vanillin, which was synergism in nature. A high inhibition efficiency, 98% was obtained by a mixture of 25-200 mg l -1 vanillin and 300-475 mg l -1 Ce 4+ . UV-vis showed that the new complex of Ce 4+ -vanillin was formed in 1.0 M H 2 SO 4 for Ce 4+ combination with vanillin. Polarization studies showed that the complex of Ce 4+ -vanillin acted as a mixed-type inhibitor, which drastically inhibits both anodic and cathodic reactions. FTIR and XPS revealed that a protective film formed in the presence of both vanillin and Ce 4+ was composed of cerium oxide and the complex of Ce 4+ -vanillin. The synergism between Ce 4+ and vanillin could also be evidenced by AFM images. Depending on the results, the synergism mechanism was discussed

  14. Error mapping of high-speed AFM systems

    Science.gov (United States)

    Klapetek, Petr; Picco, Loren; Payton, Oliver; Yacoot, Andrew; Miles, Mervyn

    2013-02-01

    In recent years, there have been several advances in the development of high-speed atomic force microscopes (HSAFMs) to obtain images with nanometre vertical and lateral resolution at frame rates in excess of 1 fps. To date, these instruments are lacking in metrology for their lateral scan axes; however, by imaging a series of two-dimensional lateral calibration standards, it has been possible to obtain information about the errors associated with these HSAFM scan axes. Results from initial measurements are presented in this paper and show that the scan speed needs to be taken into account when performing a calibration as it can lead to positioning errors of up to 3%.

  15. High-resolution retinal imaging using adaptive optics and Fourier-domain optical coherence tomography

    Science.gov (United States)

    Olivier, Scot S.; Werner, John S.; Zawadzki, Robert J.; Laut, Sophie P.; Jones, Steven M.

    2010-09-07

    This invention permits retinal images to be acquired at high speed and with unprecedented resolution in three dimensions (4.times.4.times.6 .mu.m). The instrument achieves high lateral resolution by using adaptive optics to correct optical aberrations of the human eye in real time. High axial resolution and high speed are made possible by the use of Fourier-domain optical coherence tomography. Using this system, we have demonstrated the ability to image microscopic blood vessels and the cone photoreceptor mosaic.

  16. Full-field parallel interferometry coherence probe microscope for high-speed optical metrology.

    Science.gov (United States)

    Safrani, A; Abdulhalim, I

    2015-06-01

    Parallel detection of several achromatic phase-shifted images is used to obtain a high-speed, high-resolution, full-field, optical coherence probe tomography system based on polarization interferometry. The high enface imaging speed, short coherence gate, and high lateral resolution provided by the system are exploited to determine microbump height uniformity in an integrated semiconductor chip at 50 frames per second. The technique is demonstrated using the Linnik microscope, although it can be implemented on any polarization-based interference microscopy system.

  17. Synthesis, structural, X-ray photoelectron spectroscopy (XPS) studies and IR induced anisotropy of Tl{sub 4}HgI{sub 6} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Parasyuk, O.V. [Department of Inorganic and Physical Chemistry, Lesya Ukrainka Eastern European National University, Voli Ave. 13, Lutsk, 43025 (Ukraine); Khyzhun, O.Y. [Frantsevych Institute for Problems of Materials Science, National Academy of Sciences of Ukraine, 3 Krzhyzhanivsky St., 03142, Kyiv (Ukraine); Piasecki, M. [Institute of Physics, J. Dlugosz University Częstochowa, Armii Krajowej 13/15, Częstochowa (Poland); Kityk, I.V., E-mail: iwank74@gmail.com [Electrical Engineering Department, Czestochowa University Technology, Armii Krajowej 17, PL-42-217, Czestochowa (Poland); Lakshminarayana, G. [Wireless and Photonic Networks Research Centre, Faculty of Engineering, Universiti Putra Malaysia, 43400, Serdang, Selangor (Malaysia); Luzhnyi, I. [Frantsevych Institute for Problems of Materials Science, National Academy of Sciences of Ukraine, 3 Krzhyzhanivsky St., 03142, Kyiv (Ukraine); Fochuk, P.M. [Yuriy Fed’kovych Chernivtsi National University, 2 Kotziubynskoho Str., 58012, Chernivtsi (Ukraine); Fedorchuk, A.O. [Department of Inorganic and Organic Chemistry, Lviv National University of Veterinary Medicine and Biotechnologies, Pekarska Street 50, 79010, Lviv (Ukraine); Levkovets, S.I.; Yurchenko, O.M.; Piskach, L.V. [Department of Inorganic and Physical Chemistry, Lesya Ukrainka Eastern European National University, Voli Ave. 13, Lutsk, 43025 (Ukraine)

    2017-02-01

    In the present work, we report on the synthesis and structural properties including X-ray protoelectron spectroscopy (XPS) analysis of Tl{sub 4}HgI{sub 6} crystals that were grown by Bridgman-Stockbarger method up to 80 mm in length and 18 mm in diameter. The existence of the ternary compound Tl{sub 4}HgI{sub 6} that melts incongruently at 641 K was confirmed. Phase equilibria and structural properties for the TlI–HgI{sub 2} system were investigated by differential thermal analysis (DTA) and X-ray diffraction (XRD) methods. X-ray photoelectron spectra were measured for both pristine and Ar{sup +} ion-bombarded Tl{sub 4}HgI{sub 6} single crystal surfaces. The data reveal that the Tl{sub 4}HgI{sub 6} single crystal is sensitive with respect to Ar{sup +} ion-bombardment as 3.0 keV Ar{sup +} irradiation over 5 min at an ion current density 14 μA/cm{sup 2} induces changes to the elemental stoichiometry of the Tl{sub 4}HgI{sub 6} surface, leading to a decrease of the mercury content in the topmost surface layers. X-ray photoelectron spectroscopy (XPS) measurements indicate very low hygroscopic nature of the Tl{sub 4}HgI{sub 6} single crystal surface. The IR coherent bicolor laser treatment at wavelengths 10.6/5.3 μm has shown an occurrence of anisotropy at wavelengths 1540 nm of Er:glass laser. This may open the applications of Tl{sub 4}HgI{sub 6} as a material for IR laser triggering. - Highlights: • Phase diagram of the HgI{sub 2}–TlI system was built. • Tl{sub 4}HgI{sub 6} single crystals were grown by Bridgman Stockbarger method. • XRD, XPS analysis was done. • Ir induced anisotropy was established. • The compounds may be proposed as Ir laser operated polarizers.

  18. XPS and NRA investigations during the fabrication of gold nanostructured functionalized screen-printed sensors for the detection of metallic pollutants

    International Nuclear Information System (INIS)

    Jasmin, Jean-Philippe; Miserque, Frédéric; Dumas, Eddy; Vickridge, Ian; Ganem, Jean-Jacques; Cannizzo, Caroline; Chaussé, Annie

    2017-01-01

    Highlights: • Functionalized nanostructured SPEs were made by multi-step diazonium salt chemistry. • Investigation of SPEs surface by XPS and NRA shows monolayer coverage by aminobenzyl groups. • Complete conversion of aminobenzyl groups into diazonium functions was also evidenced. • Covalent grafting of AuNPs onto SPEs lead to an unusual modification of Au-4f core level spectrum. • Ligand and lead signals showed the interest of nanostructurated SPEs for trace metals detection. - Abstract: An all covalent nanostructured lead sensor was built by the successive grafting of gold nanoparticles and carboxylic ligands at the surface of self-adhesive carbon screen-printed electrodes (SPEs). Surface analysis techniques were used in each step in order to investigate the structuration of this sensor. The self-adhesive surfaces were made from the electrochemical grafting of p-phenylenediamine at the surface of the SPEs via diazonium salts chemistry. The quantity of grafted aniline functions, estimated by Nuclear Reaction Analysis (NRA) performed with p-phenylenediamine labelled with "1"5N isotope, is in agreement with an almost complete coverage of the electrode surface. The subsequent diazotization of the aniline functions at the surface of the SPEs was performed; X-ray Photoelectron Spectroscopy (XPS) allowed us to consider a quantitative conversion of the aniline functions into diazonium moieties. The spontaneous grafting of gold nanoparticles on the as-obtained reactive surfaces ensures the nanostructuration of the material, and XPS studies showed that the covalent bonding of the gold nanoparticles at the surface of the SPEs induces a change both in the Au-4f (gold nanoparticles) and Cl-2p (carbon ink) core level signals. These unusual observations are explained by an interaction between the carbon ink constituting the substrate and the gold nanoparticles. Heavy and toxic metals are considered of major environmental concern because of their non

  19. XPS and NRA investigations during the fabrication of gold nanostructured functionalized screen-printed sensors for the detection of metallic pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Jasmin, Jean-Philippe [Laboratoire Analyse et Modélisation pour la Biologie et l’Environnement, UMR 8587, CNRS-Université Evry Val d’Essonne-CEA, 1 rue du père Jarlan, 91025 Evry Cedex (France); Miserque, Frédéric [Den-Service de la Corrosion et du Comportement des Matériaux dans leur Environnement (SCCME), CEA, Université Paris-Saclay, F-91191, Gif-sur-Yvette (France); Dumas, Eddy [Institut Lavoisier de Versailles, UMR 8180, CNRS-Université de Versailles Saint-Quentin-en-Yvelines, 78035 Versailles (France); Vickridge, Ian; Ganem, Jean-Jacques [INSP, UMR 7588, CNRS- Université Pierre et Marie Curie, 4 place Jussieu, boîte courrier 840 75252 Paris, Cedex 05 (France); Cannizzo, Caroline, E-mail: caroline.cannizzo@univ-evry.fr [Laboratoire Analyse et Modélisation pour la Biologie et l’Environnement, UMR 8587, CNRS-Université Evry Val d’Essonne-CEA, 1 rue du père Jarlan, 91025 Evry Cedex (France); Chaussé, Annie [Laboratoire Analyse et Modélisation pour la Biologie et l’Environnement, UMR 8587, CNRS-Université Evry Val d’Essonne-CEA, 1 rue du père Jarlan, 91025 Evry Cedex (France)

    2017-03-01

    Highlights: • Functionalized nanostructured SPEs were made by multi-step diazonium salt chemistry. • Investigation of SPEs surface by XPS and NRA shows monolayer coverage by aminobenzyl groups. • Complete conversion of aminobenzyl groups into diazonium functions was also evidenced. • Covalent grafting of AuNPs onto SPEs lead to an unusual modification of Au-4f core level spectrum. • Ligand and lead signals showed the interest of nanostructurated SPEs for trace metals detection. - Abstract: An all covalent nanostructured lead sensor was built by the successive grafting of gold nanoparticles and carboxylic ligands at the surface of self-adhesive carbon screen-printed electrodes (SPEs). Surface analysis techniques were used in each step in order to investigate the structuration of this sensor. The self-adhesive surfaces were made from the electrochemical grafting of p-phenylenediamine at the surface of the SPEs via diazonium salts chemistry. The quantity of grafted aniline functions, estimated by Nuclear Reaction Analysis (NRA) performed with p-phenylenediamine labelled with {sup 15}N isotope, is in agreement with an almost complete coverage of the electrode surface. The subsequent diazotization of the aniline functions at the surface of the SPEs was performed; X-ray Photoelectron Spectroscopy (XPS) allowed us to consider a quantitative conversion of the aniline functions into diazonium moieties. The spontaneous grafting of gold nanoparticles on the as-obtained reactive surfaces ensures the nanostructuration of the material, and XPS studies showed that the covalent bonding of the gold nanoparticles at the surface of the SPEs induces a change both in the Au-4f (gold nanoparticles) and Cl-2p (carbon ink) core level signals. These unusual observations are explained by an interaction between the carbon ink constituting the substrate and the gold nanoparticles. Heavy and toxic metals are considered of major environmental concern because of their non

  20. Vacancy ordered γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanohydroxyapatite: XRD, FTIR, TEM, XPS and Mössbauer studies

    Energy Technology Data Exchange (ETDEWEB)

    Ramos Guivar, Juan A., E-mail: juan.ramos5@unmsm.edu.pe [Faculty of Physical Sciences, National University of San Marcos, P. O. Box 14- 0149, Lima 14 (Peru); Sanches, Edgar A., E-mail: sanches.ufam@gmail.com [Federal University of Amazonas, Department of Physics, Manaus/AM (Brazil); Bruns, Florian, E-mail: f.bruns@tu-braunschweig.de [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Sadrollahi, Elaheh, E-mail: elahe.sadrollahi@gmail.com [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Morales, M.A., E-mail: marco.moralestorres@gmail.com [Department of Theoretical and Experimental Physics, UFRN, Natal, RN 59078- 970 (Brazil); López, Elvis O., E-mail: lopmezel@gmail.com [Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil); Litterst, F. Jochen, E-mail: litterst@cbpf.br [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil)

    2016-12-15

    Graphical abstract: Possible bonding configuration in the γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanoHAp. - Highlights: • Coprecipitation in alkaline medium for the synthesis of vacancy ordered γ-Fe{sub 2}O{sub 3}@HAp nanocomposite. • Samples were characterized by XRD, FTIR, XPS, TEM, VSM and Mössbauer spectroscopy. • The functionalization is explained with the binding of two oxygens of chemisorbed H{sub 2}O molecules at the common interface of HAp/C{sub 6}H{sub 8}O{sub 7}/γ-Fe{sub 2}O{sub 3}. - Abstract: Vacancy ordered maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles functionalized with nanohydroxyapatite (HAp – Ca{sub 10}(PO{sub 4}) {sub 6}(OH){sub 2}) have been successfully synthesized using an inexpensive co-precipitation chemical route. Evidence for the presence of vacancy order in maghemite was shown by the superstructure lines observed in X-ray diffraction. The adsorption of carboxyl groups of citric acid (C{sub 6}H{sub 8}O{sub 7}) onto γ-Fe{sub 2}O{sub 3} nanoparticles was investigated by FTIR, XPS and Mössbauer spectroscopy. From XPS surface analysis, two binding energies related to oxygen were attributed to bindings between C{sub 6}H{sub 8}O{sub 7}/γ- Fe{sub 2}O{sub 3} and C{sub 6}H{sub 8}O{sub 7}/HAp from an interfacial reaction promoted by strongly adsorbed H{sub 2}O molecules at the surface of these nanomaterials. Le Bail refinement of the XRD patterns showed the formation of well-crystallized pure tetragonal maghemite before and after functionalization with nanoHAp. The temperature dependence of hyperfine parameters of pure and functionalized γ-Fe{sub 2}O{sub 3} nanoparticles was investigated via Mössbauer spectroscopy. TEM revealed the formation of quasi-spherical γ- Fe{sub 2}O{sub 3} nanoparticles with an average diameter of ca. 12 nm and 16 nm before and after functionalization with nanoHAp in agreement with Le Bail refinement. Magnetometry measurements showed a saturation magnetization of 12 emu/g and a blocking

  1. The surface chemistry of nanocrystalline MgO catalysts for FAME production: An in situ XPS study of H2O, CH3OH and CH3OAc adsorption

    Science.gov (United States)

    Montero, J. M.; Isaacs, M. A.; Lee, A. F.; Lynam, J. M.; Wilson, K.

    2016-04-01

    An in situ XPS study of water, methanol and methyl acetate adsorption over as-synthesised and calcined MgO nanocatalysts is reported with a view to gaining insight into the surface adsorption of key components relevant to fatty acid methyl esters (biodiesel) production during the transesterification of triglycerides with methanol. High temperature calcined NanoMgO-700 adsorbed all three species more readily than the parent material due to the higher density of electron-rich (111) and (110) facets exposed over the larger crystallites. Water and methanol chemisorb over the NanoMgO-700 through the conversion of surface O2 - sites to OH- and coincident creation of Mg-OH or Mg-OCH3 moieties respectively. A model is proposed in which the dissociative chemisorption of methanol occurs preferentially over defect and edge sites of NanoMgO-700, with higher methanol coverages resulting in physisorption over weakly basic (100) facets. Methyl acetate undergoes more complex surface chemistry over NanoMgO-700, with C-H dissociation and ester cleavage forming surface hydroxyl and acetate species even at extremely low coverages, indicative of preferential adsorption at defects. Comparison of C 1s spectra with spent catalysts from tributyrin transesterification suggest that ester hydrolysis plays a key factor in the deactivation of MgO catalysts for biodiesel production.

  2. XPS study on Mg0.9-xTi0.1PdxNi (x = 0.04, 0.06, 0.08, 0.1) hydrogen storage electrode alloys after charge-discharge cycles

    International Nuclear Information System (INIS)

    Tian Qifeng; Zhang Yao; Wu Yuanxin

    2009-01-01

    The passive film composition of Mg 0.9-x Ti 0.1 Pd x Ni (x = 0.04, 0.06, 0.08, 0.1) hydrogen storage alloys after 40 charge-discharge cycles has been investigated by means of X-ray photoelectron spectroscopy (XPS) in combination with Ar + sputtering technology. With the XPSPEAK software, high resolution spectra of alloy elements and oxygen were deconvolved into individual peaks. Composites formed by metal elements and their relative contents were also deduced. It was found that the composites originated from Mg and Ni were mainly in the form of their oxides and hydroxides, which existed at the top surface of alloys. With the increase of sputtering depth, the hydroxides of Mg and Ni gradually disappeared while corresponding oxides dominated their passive products. According to the analysis results of oxygen spectra, the elemental segregation of Mg and Ni was influenced by the substitution of Pd because the addition of Pd slightly enhanced the surface energy of the alloys and suppressed the formation of Mg hydroxide and oxide. Ti and Pd presented multiple-oxides from the surface to the inner alloys and metallic Pd appeared in the sub-layers of the alloys' surface. The possible mechanisms of the formation of passive products were suggested on the basis of the discussion in the paper.

  3. Energy-filtered Photoelectron Emission Microscopy (EF-PEEM) for imaging nanoelectronic materials

    International Nuclear Information System (INIS)

    Renault, Olivier; Chabli, Amal

    2007-01-01

    Photoelectron-Emission Microscopy (PEEM) is the most promising approach to photoemission-based (XPS, UPS) imaging techniques with high lateral resolution, typically below 100 nm. It has now reached its maturity with a new generation of instruments with energy-filtering capabilities. Therefore UPS and XPS imaging with energy-filtered PEEM (EF-PEEM) can be applied to technologically-relevant samples. UPS images with contrast in local work function, obtained with laboratory UV sources, are obtained in ultra-high vacuum environment with lateral resolutions better than 50 nm and sensitivies of 20 meV. XPS images with elemental and bonding state contrast can show up lateral resolution better than 200 nm with synchrotron excitation. In this paper, we present the principles and capabilities of EF-PEEM and nanospectroscopy. Then, we focus on an example of application to non-destructive work-function imaging of polycrystalline copper for advanced interconnects, where it is shown that EF-PEEM is an alternative to Kelvin probes

  4. Breakdown of the one-electron picture in XPS, XES and AES spectra involving 4s and 4p holes in Pd to Xe

    International Nuclear Information System (INIS)

    Ohno, M.; Wendin, G.

    1981-01-01

    Certain XES spectra of Pd to Xe have been calculated using diagrammatic many-body theory within the framework of a free atom calculation. Both XPS an XES spectra demonstrate breakdown of the one-electron picture of a 4p hole due to strong dynamical grant-Coster Kronig (gCK) fluctuation and decay processes. For a 4s hole, there is a large energy shift due to gCK fluctuation, but an effective one-electron model of the 4s hole is valid. For elements Cd to Te, gCK fluctuation and decay lead to broad continuance spectrum and breakdown of the 4p model. Breakdown of the one-electron, or even quasi-particle, model must occur when 4s and 4p holes are part of multiple vacancies

  5. Application of XPS and nuclear technique to the study of the gel layers formed under different redex conditions on leached glasses

    International Nuclear Information System (INIS)

    Manara, A.; Lanza, F.; Ceccone, G.; Della Mea, G.; Salvagno, G.

    1984-01-01

    Surface analysis has been conducted on samples leached in a Soxhlet apparatus at 100 0 C in presence and in absence of air. The XPS and RBS techniques were applied to analyse the content of the silicon, iron and uranium while the nuclear reaction method was utilized to analyse the hydrogen content. The anoxic environment favors the release of iron while decreasing the dissolution of uranium. Hydrogen content is always higher in samples leached in presence of air. Silicon depletion is evident in all cases. The diffusion process seems to regulate the growth of the layer on the glass surface. After long leaching time a detachment, at least partial, of this layer is observed. 14 refs., 9 figs., 1 tab

  6. XPS Study of Chemical Changes on the La/Ce Treated Surface of A361 Aluminium Alloy Exposed to Air at Temperatures up to 500∘C

    Directory of Open Access Journals (Sweden)

    A. Pardo

    2009-01-01

    Full Text Available The chemical changes that take place on the rare earth treated surface of the A361 aluminium alloy exposed to air at temperatures between 100 and 500∘C have been examined using X-ray photoelectron spectroscopy (XPS. The most notable features discussed in this work are the disappearance of Mg and Si signals at the tested temperatures and disappearance of the Ce signal at temperatures of 400–500∘C. The biphasic microstructure of the A361 alloy, constituted by close to 12 wt% Si and the Al matrix, plays an important role in many of the results obtained. The notable growth of aluminium oxide across the conversion coating in the case of the Ce-treated surface is related to the structural transformation experienced by the cerium oxide coating at 400–500∘C.

  7. Effect of nitrogen plasma afterglow on the surface charge effect resulted during XPS surface analysis of amorphous carbon nitride thin films

    Science.gov (United States)

    Kayed, Kamal

    2018-06-01

    The aim of this paper is to investigate the relationship between the micro structure and the surface charge effect resulted during XPS surface analysis of amorphous carbon nitride thin films prepared by laser ablation method. The study results show that the charge effect coefficient (E) is not just a correction factor. We found that the changes in this coefficient value due to incorporation of nitrogen atoms into the carbon network are related to the spatial configurations of the sp2 bonded carbon atoms, order degree and sp2 clusters size. In addition, results show that the curve E vs. C(sp3)-N is a characteristic curve of the micro structure. This means that using this curve makes it easy to sorting the samples according to the micro structure (hexagonal rings or chains).

  8. High resolution eddy current microscopy

    Science.gov (United States)

    Lantz, M. A.; Jarvis, S. P.; Tokumoto, H.

    2001-01-01

    We describe a sensitive scanning force microscope based technique for measuring local variations in resistivity by monitoring changes in the eddy current induced damping of a cantilever with a magnetic tip oscillating above a conducting sample. To achieve a high sensitivity, we used a cantilever with an FeNdBLa particle mounted on the tip. Resistivity measurements are demonstrated on a silicon test structure with a staircase doping profile. Regions with resistivities of 0.0013, 0.0041, and 0.022 Ω cm are clearly resolved with a lateral resolution of approximately 180 nm. For this range of resistivities, the eddy current induced damping is found to depend linearly on the sample resistivity.

  9. Corrosion inhibition performance of 2,5-bis(4-dimethylaminophenyl)-1,3,4-oxadiazole for carbon steel in HCl solution: Gravimetric, electrochemical and XPS studies

    Energy Technology Data Exchange (ETDEWEB)

    Bouanis, M.; Tourabi, M.; Nyassi, A. [Laboratoire de Catalyse et de Corrosion des Matériaux (LCCM), Faculté des Sciences, Université Chouaib Doukkali, B.P. 20, M-24000 El Jadida (Morocco); Zarrouk, A. [LCAE-URAC 18, Faculty of Science, First Mohammed University, PO Box 717, M-60 000 Oujda (Morocco); Jama, C. [UMET-ISP, CNRS UMR 8207, ENSCL, Université Lille Nord de France, CS 90108, F-59652 Villeneuve d' Ascq Cedex (France); Bentiss, F., E-mail: fbentiss@gmail.com [Laboratoire de Catalyse et de Corrosion des Matériaux (LCCM), Faculté des Sciences, Université Chouaib Doukkali, B.P. 20, M-24000 El Jadida (Morocco); UMET-ISP, CNRS UMR 8207, ENSCL, Université Lille Nord de France, CS 90108, F-59652 Villeneuve d' Ascq Cedex (France)

    2016-12-15

    Highlights: • 2,5-Bis(4-dimethylaminophenyl)-1,3,4-oxadiazole is good corrosion inhibitor for carbon steel in 1 M HCl. • XPS analysis has provided the composition of adsorbed protective layer on the steel surface. • The adsorption of the investigated 1,3,4-oxadiazole is mainly due to chemisorption. - Abstract: Corrosion inhibition of carbon steel in normal hydrochloric acid solution at 30 °C by 2,5-bis(4-dimethylaminophenyl)-1,3,4-oxadiazole (DAPO) has been studied by weight loss measurements and electrochemical techniques (polarization and AC impedance). The experimental results showed that DAPO acted as an efficient inhibitor against the carbon steel corrosion in 1 M HCl, and its inhibition efficiency increased with the inhibitor concentration reaching a value up to 93% at 1 mM. Polarization studies showed that the DAPO was a mixed-type inhibitor. The adsorption of this 1,3,4-oxadiazole derivative on the carbon steel surface in 1 M HCl solution followed the Langmuir adsorption isotherm and the corresponding value of the standard Gibbs free energy of adsorption (ΔG°{sub ads}) is associated to a chemisorption mechanism. Scanning Electron Microscopy (SEM) and X-Ray Photoelectron Spectroscopy (XPS) analyses were carried out to characterize the chemical composition of the inhibitive film formed on the steel surface. The surfaces studies showed that the inhibitive layer is composed of an iron oxide/hydroxide mixture where DAPO molecules are incorporated. The cytotoxicity of DAPO was also determined using cell culture system.

  10. New 1H-pyrrole-2,5-dione derivatives as efficient organic inhibitors of carbon steel corrosion in hydrochloric acid medium: Electrochemical, XPS and DFT studies

    International Nuclear Information System (INIS)

    Zarrouk, A.; Hammouti, B.; Lakhlifi, T.; Traisnel, M.; Vezin, H.; Bentiss, F.

    2015-01-01

    Highlights: • 1H-pyrrole derivatives act as good corrosion inhibitors for carbon steel in 1 M HCl. • Adsorption of the inhibitors on carbon steel surface obeys Langmuir’s isotherm. • XPS showed that the inhibitors are chemisorbed on the metal surface. • Quantum chemical parameters were correlated with experimental results. - Abstract: New 1H-pyrrole-2,5-dione derivatives, namely 1-phenyl-1H-pyrrole-2,5-dione (PPD) and 1-(4-methylphenyl)-1H-pyrrole-2,5-dione (MPPD) were synthesised and their inhibitive action against the corrosion of carbon steel in 1 M HCl solution were investigated at 308 K by weight loss, potentiodynamic polarization curves, and electrochemical impedance spectroscopy (EIS) methods. The results showed that the investigated 1H-pyrrole-2,5-dione derivatives are good corrosion inhibitors for carbon steel in 1 M HCl medium, their inhibition efficiency increased with inhibitor concentration, and MPPD is slightly more effective than PPD. Potentiostatic polarization study showed that PPD and MPPD are mixed-type inhibitors in 1 M HCl. Impedance experimental data revealed a frequency distribution of the capacitance, simulated as constant phase element. The results obtained from electrochemical and weight loss studies were in reasonable agreement. The adsorption of MPPD and PPD on steel surface obeyed Langmuir’s adsorption isotherm. Thermodynamic data and XPS analysis clearly indicated that the adsorption mechanism of 1H-pyrrole-2,5-dione derivatives on carbon steel surface in 1 M HCl solution is mainly controlled by a chemisorption process. Quantum chemical calculations using the Density Functional Theory (DFT) were performed on 1H-pyrrole-2,5-dione derivatives to determine the relationship between molecular structures and their inhibition efficiencies

  11. XPS and NRA investigations during the fabrication of gold nanostructured functionalized screen-printed sensors for the detection of metallic pollutants

    Science.gov (United States)

    Jasmin, Jean-Philippe; Miserque, Frédéric; Dumas, Eddy; Vickridge, Ian; Ganem, Jean-Jacques; Cannizzo, Caroline; Chaussé, Annie

    2017-03-01

    An all covalent nanostructured lead sensor was built by the successive grafting of gold nanoparticles and carboxylic ligands at the surface of self-adhesive carbon screen-printed electrodes (SPEs). Surface analysis techniques were used in each step in order to investigate the structuration of this sensor. The self-adhesive surfaces were made from the electrochemical grafting of p-phenylenediamine at the surface of the SPEs via diazonium salts chemistry. The quantity of grafted aniline functions, estimated by Nuclear Reaction Analysis (NRA) performed with p-phenylenediamine labelled with 15N isotope, is in agreement with an almost complete coverage of the electrode surface. The subsequent diazotization of the aniline functions at the surface of the SPEs was performed; X-ray Photoelectron Spectroscopy (XPS) allowed us to consider a quantitative conversion of the aniline functions into diazonium moieties. The spontaneous grafting of gold nanoparticles on the as-obtained reactive surfaces ensures the nanostructuration of the material, and XPS studies showed that the covalent bonding of the gold nanoparticles at the surface of the SPEs induces a change both in the Au-4f (gold nanoparticles) and Cl-2p (carbon ink) core level signals. These unusual observations are explained by an interaction between the carbon ink constituting the substrate and the gold nanoparticles. Heavy and toxic metals are considered of major environmental concern because of their non-biodegradability. In a final step, the grafting of the carboxylic ligands at the surface of the SPEs and an accumulation step in the presence of lead(II) cations allowed us to evidence the interest of nanostructured materials as metallic pollutants sensors.

  12. Proton transfer and hydrogen bonding in the organic solid state: a combined XRD/XPS/ssNMR study of 17 organic acid-base complexes.

    Science.gov (United States)

    Stevens, Joanna S; Byard, Stephen J; Seaton, Colin C; Sadiq, Ghazala; Davey, Roger J; Schroeder, Sven L M

    2014-01-21

    The properties of nitrogen centres acting either as hydrogen-bond or Brønsted acceptors in solid molecular acid-base complexes have been probed by N 1s X-ray photoelectron spectroscopy (XPS) as well as (15)N solid-state nuclear magnetic resonance (ssNMR) spectroscopy and are interpreted with reference to local crystallographic structure information provided by X-ray diffraction (XRD). We have previously shown that the strong chemical shift of the N 1s binding energy associated with the protonation of nitrogen centres unequivocally distinguishes protonated (salt) from hydrogen-bonded (co-crystal) nitrogen species. This result is further supported by significant ssNMR shifts to low frequency, which occur with proton transfer from the acid to the base component. Generally, only minor chemical shifts occur upon co-crystal formation, unless a strong hydrogen bond is formed. CASTEP density functional theory (DFT) calculations of (15)N ssNMR isotropic chemical shifts correlate well with the experimental data, confirming that computational predictions of H-bond strengths and associated ssNMR chemical shifts allow the identification of salt and co-crystal structures (NMR crystallography). The excellent agreement between the conclusions drawn by XPS and the combined CASTEP/ssNMR investigations opens up a reliable avenue for local structure characterization in molecular systems even in the absence of crystal structure information, for example for non-crystalline or amorphous matter. The range of 17 different systems investigated in this study demonstrates the generic nature of this approach, which will be applicable to many other molecular materials in organic, physical, and materials chemistry.

  13. Morphology and chemical characteristics of micro- and Nano-particles in the haze in Beijing studied by XPS and TEM/EDX

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Peng [Beijing Key Laboratory for Green Catalysis and Separation, Key Laboratory of Beijing on Regional Air Pollution Control, Key Laboratory of Advanced Functional Materials, Education Ministry of China, and Laboratory of Catalysis Chemistry and Nanoscience, Department of Chemistry and Chemical Engineering, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124 (China); CAS Key Laboratory of Standardization and Measurement for Nanotechnology, National Center for Nanoscience and Technology, Beijing, 100190 (China); Xu, Jianxun; He, Meng [CAS Key Laboratory of Standardization and Measurement for Nanotechnology, National Center for Nanoscience and Technology, Beijing, 100190 (China); Song, Lexin [Department of Chemistry, University of Science and Technology of China, Hefei, 230026 (China); Chen, Dongliang, E-mail: chendl@mail.buct.edu.cn [College of Mechanical and Electrical Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Guo, Guangsheng, E-mail: guogs@bjut.edu.cn [Beijing Key Laboratory for Green Catalysis and Separation, Key Laboratory of Beijing on Regional Air Pollution Control, Key Laboratory of Advanced Functional Materials, Education Ministry of China, and Laboratory of Catalysis Chemistry and Nanoscience, Department of Chemistry and Chemical Engineering, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124 (China); Dai, Hongxing, E-mail: hxdai@bjut.edu.cn [Beijing Key Laboratory for Green Catalysis and Separation, Key Laboratory of Beijing on Regional Air Pollution Control, Key Laboratory of Advanced Functional Materials, Education Ministry of China, and Laboratory of Catalysis Chemistry and Nanoscience, Department of Chemistry and Chemical Engineering, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124 (China)

    2016-09-15

    X-ray Photoelectron Spectroscopy (XPS) is a useful surface sensitive tool to explore the particulate matter with different particle sizes. In this work, we report the analysis of elemental species in particulate matter with size ranging from 100 nm to 10 μm during the autumn haze of 2014 in Beijing. The size dependence of element composition and chemical state distribution on the particle surface was investigated. It was found that the number of investigated element species decreased from 8 (at stage 2) to 4 (at stage 10) with the decrease of particle sizes down to 100 nm, which is in accordance with the result from Transmission electron microscopy (TEM/EDX) observations. Three chemical states of nitrogen, the amide group (399.9 eV), the ammonium group (401.6 eV), and the nitrate group (407.2 eV), were confirmed according to the different binding energies. Nitrate was the main composition on the coarse particles, while the percentage of amide and ammonium at stage 3 (13.9% and 10.8% respectively) increased on the fine particles at stage 9 (46.8% and 38.8% respectively). The relative ratio of sulfate and ammonium (calculated 1:1) in the fine particles suggests that there is no enough NH{sub 4}{sup +} to neutralize the sulfuric acid and the surface of the PM is acidic. The result is useful to investigate the generation processes and the sources of collected particles. - Highlights: • The element composition of particles from 100 nm to 10 μm in haze was discussed • The chemical state was dominated by the particle size • The surface of PM was acidity • XPS was shown a useful tool in the aerosol research.

  14. Analysis of buried interfaces in multilayer device structures with hard XPS (HAXPES) using a CrKα source

    DEFF Research Database (Denmark)

    Renault, O.; Martinez, E.; Zborowski, C.

    2018-01-01

    Applications of laboratory hard X-ray photoelectron spectroscopy on buried interfaces in devices are presented. We use a novel spectrometer fitted with a monochromated CrKα source (photon energy: 5414.9 eV) and a high-voltage analyzer. Elements buried at depths as deep as 25 nm underneath various...

  15. Surface characterization of insulin-coated Ti6Al4V medical implants conditioned in cell culture medium: An XPS study

    Energy Technology Data Exchange (ETDEWEB)

    Shchukarev, Andrey, E-mail: andrey.shchukarev@umu.se [Department of Chemistry, Umeå University, Umeå SE-90187 (Sweden); Malekzadeh, Behnosh Öhrnell [Department of Orthodontics, Institute of Odontology, Sahlgrenska Academy, University of Gothenburg, SE-40530 (Sweden); Department of Biomaterials, Institute of Clinical Sciences, Sahlgrenska Academy, University of Gothenburg, SE-40530 (Sweden); Ransjö, Maria [Department of Orthodontics, Institute of Odontology, Sahlgrenska Academy, University of Gothenburg, SE-40530 (Sweden); Tengvall, Pentti [Department of Biomaterials, Institute of Clinical Sciences, Sahlgrenska Academy, University of Gothenburg, SE-40530 (Sweden); Westerlund, Anna [Department of Orthodontics, Institute of Odontology, Sahlgrenska Academy, University of Gothenburg, SE-40530 (Sweden)

    2017-04-15

    Highlights: • In the absence of FBS, chemically immobilized insulin layer remains intact; • The immobilized insulin expose hydrophobic domains outward the implant; • In the presence of FBS, a partial replacement of insulin occurs; • The immobilized insulin stabilizes the secondary structure of adsorbed proteins. - Abstract: Surface characterization of insulin-coated Ti6Al4V medical implants, after incubation in α-minimum essential medium (α-MEM), was done by X-ray photoelectron spectroscopy (XPS), in order to analyze the insulin behavior at the implant – α-MEM interface. In the absence of serum proteins in cell culture medium, the coated insulin layer remained intact, but experienced a time-dependent structural transformation exposing hydrophobic parts of the protein toward the solution. The presence of fetal bovine serum (FBS) in the medium resulted in partial substitution of insulin by serum proteins. In spite of some insulin release, the remaining coated layer demonstrated a direct surface effect by stabilizing the structure of protein competitors, and by supporting the accumulation of calcium and phosphate ions at the interface. A structurally stable protein layer with incorporated calcium and phosphate ions at the implant–tissue interface could be an important prerequisite for enhanced bone formation.

  16. XPS analysis and structural and morphological characterization of Cu{sub 2}ZnSnS{sub 4} thin films grown by sequential evaporation

    Energy Technology Data Exchange (ETDEWEB)

    Gordillo, G. [Departamento de Física, Universidad Nacional de Colombia, Bogotá (Colombia); Calderón, C., E-mail: clcalderont@unal.edu.co [Departamento de Física, Universidad Nacional de Colombia, Bogotá (Colombia); Bartolo-Pérez, P. [Departamento de Física Aplicada, CINVESTAV-IPN, Mérida, Yuc. (Mexico)

    2014-06-01

    This work describes a procedure to grow single phase Cu{sub 2}ZnSnS{sub 4} (CZTS) thin films with tetragonal-kesterite type structure, through sequential evaporation of the elemental metallic precursors under sulphur vapor supplied from an effusion cell. X-ray diffraction analysis (XRD) is mostly used for phase identification but cannot clearly distinguish the formation of secondary phases such as Cu{sub 2}SnS{sub 3} (CTS) because both compounds have the same diffraction pattern; therefore the use of a complementary technique is needed. Raman scattering analysis was used to distinguish these phases. The influence of the preparation conditions on the morphology and phases present in CZTS thin films were investigated through measurements of scanning electron microscopy (SEM) and XRD, respectively. From transmittance measurements, the energy band gap of the CZTS films was estimated to be around 1.45 eV. The limitation of XRD to identify some of the remaining phases after the growth process are investigated and the results of Raman analysis on the phases formed in samples grown by this method are presented. Further, the influence of the preparation conditions on the homogeneity of the chemical composition in the volume was studied by X-ray photoelectron spectroscopy (XPS) analysis.

  17. (001) 3C SiC/Ni contact interface: In situ XPS observation of annealing induced Ni2Si formation and the resulting barrier height changes

    Science.gov (United States)

    Tengeler, Sven; Kaiser, Bernhard; Chaussende, Didier; Jaegermann, Wolfram

    2017-04-01

    The electronic states of the (001) 3C SiC/Ni interface prior and post annealing are investigated via an in situ XPS interface experiment, allowing direct observation of the induced band bending and the transformation from Schottky to ohmic behaviour for the first time. A single domain (001) 3C SiC sample was prepared via wet chemical etching. Nickel was deposited on the sample in multiple in situ deposition steps via RF sputtering, allowing observation of the 3C SiC/Ni interface formation. Over the course of the experiments, an upward band bending of 0.35 eV was observed, along with defect induced Fermi level pinning. This indicates a Schottky type contact behaviour with a barrier height of 0.41 eV. The subsequent annealing at 850 °C for 5 min resulted in the formation of a Ni2Si layer and a reversal of the band bending to 0.06 eV downward. Thus explaining the ohmic contact behaviour frequently reported for annealed n-type 3C SiC/Ni contacts.

  18. Physical aspects of relaxation and shake-up effects in XPS and core →2π* absorption spectra of CO chemisorbed on Ni (111)

    International Nuclear Information System (INIS)

    Gumhalter, B.

    1985-07-01

    The physical origin of the peculiar relaxation shifts and spectral shapes appearing in x-ray induced core-to-valence excitation and core level photoemission spectra of CO chemisorbed on Ni(111) are discussed and interpreted within a unique framework. Within the model presented the electronic transitions in core-to-valence excitation spectroscopy and XPS are shown to give rise to drastic electronic rearrangements within the adsorption system and to the charge shake-up in the CO 2π* derived resonance partly filled via the backdonation mechanism. Such singular relaxation processes, common to both spectroscopies, are closely related and can be treated on the same footing. This makes possible to establish unique relaxation shifts and spectral characteristics for two seemingly different experimental situations. The use of this formalism in analysing the experimental data enables one to estimate and distinguish between the extra-adsorbate (image or nonbonding) and intra-adsorbate (chemically induced) screening of the core holes created either by x-ray induced core-to-valence electronic transitions or core level photoionization in CO/Ni(111). (author)

  19. Electronic structure of Ar{sup +} ion-sputtered thin-film MoS{sub 2}: A XPS and IPES study

    Energy Technology Data Exchange (ETDEWEB)

    Santoni, Antonino, E-mail: antonino.santoni@enea.it [Department FSN-TECFIS-MNF, ENEA, Frascati Research Center, via E. Fermi 45, 00044 Frascati (Italy); Rondino, Flaminia [Department FSN-TECFIS-MNF, ENEA, Frascati Research Center, via E. Fermi 45, 00044 Frascati (Italy); Malerba, Claudia [Department DTE-FSN-TEF, ENEA, Casaccia Research Center, via Anguillarese 301, 00123, Roma (Italy); DICAM, University of Trento, via Mesiano 77, 38123, Trento (Italy); Valentini, Matteo [Department DTE-FSN-TEF, ENEA, Casaccia Research Center, via Anguillarese 301, 00123, Roma (Italy); Department of Physics, University of Rome “Sapienza”, P.le Aldo Moro 5, 00156 Roma (Italy); Mittiga, Alberto [Department DTE-FSN-TEF, ENEA, Casaccia Research Center, via Anguillarese 301, 00123, Roma (Italy)

    2017-01-15

    Polycrystalline MoS{sub 2} grown by Mo sulphurization was exposed to increasing doses of Ar{sup +} ions at 250 eV starting from 2.2 × 10{sup 15} ions/cm{sup 2} to 3.92 × 10{sup 17} ions/cm{sup 2}. Electronic structure changes were monitored by X-Ray Photoelectron Spectroscopy (XPS) and Inverse Photolectron Spectroscopy (IPES). No change in the Fermi level position was observed with Ar{sup +} dosing. Ion bombardment resulted in a new visible feature at lower binding energy in the Mo3d core level, while the S2p lineshape showed little changes. The formation of a steady state from 2.49 × 10{sup 17} ions/cm{sup 2} has been detected. The investigation of the occupied and unoccupied states on the steady-state surface pointed to the simultaneous presence of metallic-like Mo with amorphous MoS{sub 2-x}.

  20. Surface characterization of insulin-coated Ti6Al4V medical implants conditioned in cell culture medium: An XPS study

    International Nuclear Information System (INIS)

    Shchukarev, Andrey; Malekzadeh, Behnosh Öhrnell; Ransjö, Maria; Tengvall, Pentti; Westerlund, Anna

    2017-01-01

    Highlights: • In the absence of FBS, chemically immobilized insulin layer remains intact; • The immobilized insulin expose hydrophobic domains outward the implant; • In the presence of FBS, a partial replacement of insulin occurs; • The immobilized insulin stabilizes the secondary structure of adsorbed proteins. - Abstract: Surface characterization of insulin-coated Ti6Al4V medical implants, after incubation in α-minimum essential medium (α-MEM), was done by X-ray photoelectron spectroscopy (XPS), in order to analyze the insulin behavior at the implant – α-MEM interface. In the absence of serum proteins in cell culture medium, the coated insulin layer remained intact, but experienced a time-dependent structural transformation exposing hydrophobic parts of the protein toward the solution. The presence of fetal bovine serum (FBS) in the medium resulted in partial substitution of insulin by serum proteins. In spite of some insulin release, the remaining coated layer demonstrated a direct surface effect by stabilizing the structure of protein competitors, and by supporting the accumulation of calcium and phosphate ions at the interface. A structurally stable protein layer with incorporated calcium and phosphate ions at the implant–tissue interface could be an important prerequisite for enhanced bone formation.

  1. Surface chemical and photocatalytic consequences of Ca-doping of BiFeO{sub 3} as probed by XPS and H{sub 2}O{sub 2} decomposition studies

    Energy Technology Data Exchange (ETDEWEB)

    Zaki, Mohamed I., E-mail: mizaki@link.net [Chemistry Department, Faculty of Science, Minia University, El-Minia 61519 (Egypt); Ramadan, Wegdan [Physics Department, Faculty of Science, Alexandria University, Alexandria 21511 (Egypt); Katrib, Ali [Chemistry Department, Faculty of Science, Kuwait University, P.O. Box 5969, Safat 13060 (Kuwait); Rabee, Abdallah I.M. [Chemistry Department, Faculty of Science, Minia University, El-Minia 61519 (Egypt)

    2014-10-30

    Graphical abstract: - Highlights: • BiFeO{sub 3} is a modest visible-light heterogeneous photocatalyst for H{sub 2}O{sub 2} decomposition. • The ferrite activity is promoted with Ca-doping up to 10 wt%-Ca. • Favourable consequences are enhanced surface metal redoxability and oxide basicity. • Furthering doping to >10 wt%-Ca retrogresses the ferrite photocatalytic activity. • A retrogressive doping consequence is bulk phase separation of α(γ)-Fe{sub 2}O{sub 3}. - Abstract: Pure and Ca-doped Bi{sub 1−x}Ca{sub x}FeO{sub 3} samples were prepared with x = 0.0–0.2, adopting a sol–gel method. Previously reported studies performed on similarly composed and prepared samples revealed that Ca-doping, above solubility limit (namely at ≥10%-Ca), results in phase separation and formation of BiFeO{sub 3}/α(γ)-Fe{sub 2}O{sub 3} nanocomposite particles. Hetero p/n nanojunctions thus established were considered to help separating photo-generated electron–hole pairs and, therefore, explain consequent promotion of photo-Fenton catalytic activity of BiFeO{sub 3} towards methylene blue degradation in presence of H{sub 2}O{sub 2} additive. However, the encompassed decomposition of H{sub 2}O{sub 2} was not addressed. To bridge this gap of knowledge, the present investigation was designed to assess Ca-doping-effected surface chemical modifications and gauge its impact on the heterogeneous photo-/thermo-catalytic activity of BiFeO{sub 3} towards H{sub 2}O{sub 2} decomposition, by means of X-ray photoelectron spectroscopy (XPS) and H{sub 2}O{sub 2} decomposition gravimetry. XPS results revealed generation of high binding energy Bi 4f and Fe 2p states, as well as enhancement of the surface basicity, upon doping to 10%-Ca. These surface chemical consequences are rendered hardly detectable upon further increase of the dopant magnitude to 20%-Ca. In parallel, the H{sub 2}O{sub 2} decomposition activity of the ferrite, under natural visible light, is enhanced to optimize

  2. High-resolution multiphoton microscopy with a low-power continuous wave laser pump.

    Science.gov (United States)

    Chen, Xiang-Dong; Li, Shen; Du, Bo; Dong, Yang; Wang, Ze-Hao; Guo, Guang-Can; Sun, Fang-Wen

    2018-02-15

    Multiphoton microscopy (MPM) has been widely used for three-dimensional biological imaging. Here, based on the photon-induced charge state conversion process, we demonstrated a low-power high-resolution MPM with a nitrogen vacancy (NV) center in diamond. Continuous wave green and orange lasers were used to pump and detect the two-photon charge state conversion, respectively. The power of the laser for multiphoton excitation was 40 μW. Both the axial and lateral resolutions were improved approximately 1.5 times compared with confocal microscopy. The results can be used to improve the resolution of the NV center-based quantum sensing and biological imaging.

  3. 4. El Morchid.xps

    African Journals Online (AJOL)

    21 juin 2017 ... In order to improve their economic performance and build .... qui permet de mesurer le décalage entre l'attitude attendue des individus du ... Aussi les normes sociales sont-elles assorties d'un système de contrôle social ...... de liberté politique et les capacités de gestion macroéconomique, ils ne sont.

  4. Resolving surface chemical states in XPS analysis of first row transition metals, oxides and hydroxides: Cr, Mn, Fe, Co and Ni

    Energy Technology Data Exchange (ETDEWEB)

    Biesinger, Mark C., E-mail: biesingr@uwo.ca [Surface Science Western, University of Western Ontario, University of Western Ontario Research Park, Room LL31, 999 Collip Circle, London, Ontario, N6G 0J3 (Canada); ACeSSS (Applied Centre for Structural and Synchrotron Studies), University of South Australia, Mawson Lakes, SA 5095 (Australia); Payne, Brad P. [Department of Chemistry, University of Western Ontario, London, Ontario, N6A 5B7 (Canada); Grosvenor, Andrew P. [Department of Chemistry, University of Saskatchewan, Saskatoon, Saskatchewan, S7N 5C9 (Canada); Lau, Leo W.M. [Surface Science Western, University of Western Ontario, University of Western Ontario Research Park, Room LL31, 999 Collip Circle, London, Ontario, N6G 0J3 (Canada); Department of Chemistry, University of Western Ontario, London, Ontario, N6A 5B7 (Canada); Gerson, Andrea R.; Smart, Roger St.C. [ACeSSS (Applied Centre for Structural and Synchrotron Studies), University of South Australia, Mawson Lakes, SA 5095 (Australia)

    2011-01-15

    Chemical state X-ray photoelectron spectroscopic analysis of first row transition metals and their oxides and hydroxides is challenging due to the complexity of their 2p spectra resulting from peak asymmetries, complex multiplet splitting, shake-up and plasmon loss structure, and uncertain, overlapping binding energies. Our previous paper [M.C. Biesinger et al., Appl. Surf. Sci. 257 (2010) 887-898.] in which we examined Sc, Ti, V, Cu and Zn species, has shown that all the values of the spectral fitting parameters for each specific species, i.e. binding energy (eV), full wide at half maximum (FWHM) value (eV) for each pass energy, spin-orbit splitting values and asymmetric peak shape fitting parameters, are not all normally provided in the literature and data bases, and are necessary for reproducible, quantitative chemical state analysis. A more consistent, practical and effective approach to curve fitting was developed based on a combination of (1) standard spectra from quality reference samples, (2) a survey of appropriate literature databases and/or a compilation of literature references and (3) specific literature references where fitting procedures are available. This paper extends this approach to the chemical states of Cr, Mn, Fe, Co and Ni metals, and various oxides and hydroxides where intense, complex multiplet splitting in many of the chemical states of these elements poses unique difficulties for chemical state analysis. The curve fitting procedures proposed use the same criteria as proposed previously but with the additional complexity of fitting of multiplet split spectra which has been done based on spectra of numerous reference materials and theoretical XPS modeling of these transition metal species. Binding energies, FWHM values, asymmetric peak shape fitting parameters, multiplet peak separation and peak area percentages are presented. The procedures developed can be utilized to remove uncertainties in the analysis of surface states in nano

  5. (001) 3C SiC/Ni contact interface: In situ XPS observation of annealing induced Ni{sub 2}Si formation and the resulting barrier height changes

    Energy Technology Data Exchange (ETDEWEB)

    Tengeler, Sven, E-mail: stengeler@surface.tu-darmstadt.de [Institute of Material Science, Technische Universität Darmstadt, 64287 Darmstadt (Germany); Univ. Grenoble Alpes, CNRS, LMGP, F-38000 Grenoble (France); Kaiser, Bernhard [Institute of Material Science, Technische Universität Darmstadt, 64287 Darmstadt (Germany); Chaussende, Didier [Univ. Grenoble Alpes, CNRS, LMGP, F-38000 Grenoble (France); Jaegermann, Wolfram [Institute of Material Science, Technische Universität Darmstadt, 64287 Darmstadt (Germany)

    2017-04-01

    Highlights: • Schottky behavior (Φ{sub B} = 0.41 eV) and Fermi level pining were found pre annealing. • Ni{sub 2}Si formation was confirmed for 5 min at 850 °C. • 3C/Ni{sub 2}Si Fermi level alignment is responsible for ohmic contact behavior. • Wet chemical etching (Si–OH/C–H termination) does not impair Ni{sub 2}Si formation. - Abstract: The electronic states of the (001) 3C SiC/Ni interface prior and post annealing are investigated via an in situ XPS interface experiment, allowing direct observation of the induced band bending and the transformation from Schottky to ohmic behaviour for the first time. A single domain (001) 3C SiC sample was prepared via wet chemical etching. Nickel was deposited on the sample in multiple in situ deposition steps via RF sputtering, allowing observation of the 3C SiC/Ni interface formation. Over the course of the experiments, an upward band bending of 0.35 eV was observed, along with defect induced Fermi level pinning. This indicates a Schottky type contact behaviour with a barrier height of 0.41 eV. The subsequent annealing at 850 °C for 5 min resulted in the formation of a Ni{sub 2}Si layer and a reversal of the band bending to 0.06 eV downward. Thus explaining the ohmic contact behaviour frequently reported for annealed n-type 3C SiC/Ni contacts.

  6. (001) 3C SiC/Ni contact interface: In situ XPS observation of annealing induced Ni_2Si formation and the resulting barrier height changes

    International Nuclear Information System (INIS)

    Tengeler, Sven; Kaiser, Bernhard; Chaussende, Didier; Jaegermann, Wolfram

    2017-01-01

    Highlights: • Schottky behavior (Φ_B = 0.41 eV) and Fermi level pining were found pre annealing. • Ni_2Si formation was confirmed for 5 min at 850 °C. • 3C/Ni_2Si Fermi level alignment is responsible for ohmic contact behavior. • Wet chemical etching (Si–OH/C–H termination) does not impair Ni_2Si formation. - Abstract: The electronic states of the (001) 3C SiC/Ni interface prior and post annealing are investigated via an in situ XPS interface experiment, allowing direct observation of the induced band bending and the transformation from Schottky to ohmic behaviour for the first time. A single domain (001) 3C SiC sample was prepared via wet chemical etching. Nickel was deposited on the sample in multiple in situ deposition steps via RF sputtering, allowing observation of the 3C SiC/Ni interface formation. Over the course of the experiments, an upward band bending of 0.35 eV was observed, along with defect induced Fermi level pinning. This indicates a Schottky type contact behaviour with a barrier height of 0.41 eV. The subsequent annealing at 850 °C for 5 min resulted in the formation of a Ni_2Si layer and a reversal of the band bending to 0.06 eV downward. Thus explaining the ohmic contact behaviour frequently reported for annealed n-type 3C SiC/Ni contacts.

  7. XPS, TEM and SAD investigations of nanosized Co{sub x}B{sub y}H{sub z} particles obtained by two different borohydride methods

    Energy Technology Data Exchange (ETDEWEB)

    Krastev, V. [Bulgarian Acad. of Sci., Sofia (Bulgaria). Inst. of General and Inorg. Chem.; Stoycheva, M. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria); Lefterova, E. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria); Dragieva, I. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria); Stoynov, Z. [Central Laboratory of Electrochemical Power Sources, Bulgarian Academy of Sciences, Sofia 1113 (Bulgaria)

    1996-07-01

    The nanosized Co{sub x}B{sub y}H{sub z} particles synthesised by the ``tea`` and ``antigravity`` methods using a borohydride reduction process have been subjected to structure and composition studies by X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and selected area diffraction (SAD). The amounts of the elements Co, B, O{sub 2}, H{sub 2} and C as mean volume values, and surface values for the as-prepared particles, as well as after Ar{sup +} etching to a depth of about 15 nm and 30 nm from the initial particle surface, are determined. About 1.5 atoms of cobalt per atom of boron correspond to samples obtained by the ``antigravity`` method. The binding energy (BE) of 1s electrons of boron atoms has only one value. These particles are angular and are in the typical nanocrystalline state. In the case of samples prepared by the ``tea`` method, two atoms of cobalt per atom of boron are found. The presence of two kinds of BE (B{sup I} and B{sup II}) of 1s electrons of boron atoms in the particles obtained by the ``tea`` method is observed and almost equal amounts of these two states are established in the spectrum. The particles` shape and structure are typical of the amorphous state. The fact that there is one peak when the ``antigravity`` method is applied, in contrast to the two peaks with the ``tea`` method indicates the presence of a metal amorphous state in the latter case. (orig.)

  8. A Multi-technique Characterization of Adsorbed Protein Films: Orientation and Structure by ToF-SIMS, NEXAFS, SFG, and XPS

    Science.gov (United States)

    Baio, Joseph E.

    There are many techniques that allow surface scientists to study interfaces. However, few are routinely applied to probe biological surfaces. The work presented here demonstrates how detailed information about the conformation, orientation, chemical state, and molecular structure of biological molecules immobilized onto a surface can be assessed by electron spectroscopy, mass spectrometry, and nonlinear vibrational spectroscopy techniques. This investigation began with the development of simple model systems (small proteins, and peptides) and evolved into a study of more complex --- real world systems. Initially, two model systems based on the chemical and electrostatic immobilization of a small rigid protein (Protein G B1 domain, 6kDa) were built to develop the capabilities of time-of-flight secondary ion mass spectrometry (ToFSIMS), near edge X-ray absorption fine structure spectroscopy (NEXAFS) and sum frequency generation (SFG) spectroscopy as tools to probe the structure of surface immobilized proteins. X-ray photoelectron spectroscopy (XPS) was used to measure the amount of immobilized protein and ToF-SIMS sampled the amino acid composition of the exposed surface of the protein film. Within the ToF-SIMS spectra, an enrichment of secondary ions from amino acids located at opposite ends of the proteins were used to describe protein orientation. SFG spectral peaks characteristic of ordered alpha-helix and beta-sheet elements were observed for both systems and the phase of the peaks indicated a predominantly upright orientation for both the covalent and electrostatic configurations. Polarization dependence of the NEXAFS signal from the N 1s to pi* transition of the peptide bonds that make up the beta-sheets also indicated protein ordering at the surface. Building upon the Protein G B1 studies, the orientation and structure of a surface immobilized antibody (HuLys Fv: variant of humanized anti-lysozyme variable fragment, 26kDa) was characterized across two

  9. Identification of the silver state in the framework of Ag-containing zeolite by XRD, FTIR, photoluminescence, 109Ag NMR, EPR, DR UV-vis, TEM and XPS investigations.

    Science.gov (United States)

    Popovych, Nataliia; Kyriienko, Pavlo; Soloviev, Sergiy; Baran, Rafal; Millot, Yannick; Dzwigaj, Stanislaw

    2016-10-26

    Silver has been identified in the framework of Ag x SiBEA zeolites (where x = 3-6 Ag wt%) by the combined use of XRD, 109 Ag MAS NMR, FTIR, diffuse reflectance UV-visible, EPR and XPS spectroscopy. The incorporation of Ag ions into the framework of SiBEA zeolite has been evidenced by XRD. The consumption of OH groups as a result of their reaction with the silver precursor has been monitored by FTIR and photoluminescence spectroscopy. The changes in the silver state as a function of Ag content and thermal and hydrogen treatment at 573 K have been identified by 109 Ag MAS NMR, EPR, DR UV-visible, TEM and XPS investigations. The acidity of AgSiBEA has been investigated by FTIR spectroscopy of adsorbed CO and pyridine used as probe molecules.

  10. High-definition optical coherence tomography enables visualization of individual cells in healthy skin

    DEFF Research Database (Denmark)

    Boone, Marc; Jemec, Gregor B E; Del Marmol, Véronique

    2012-01-01

    High-definition OCT (HD-OCT) is an innovative technique based on the principle of conventional OCT. Our objective was to test the resolution and image quality of HD-OCT in comparison with reflectance confocal microscopy (RCM) of healthy skin. Firstly, images have been made of a ultra-high-resolut......High-definition OCT (HD-OCT) is an innovative technique based on the principle of conventional OCT. Our objective was to test the resolution and image quality of HD-OCT in comparison with reflectance confocal microscopy (RCM) of healthy skin. Firstly, images have been made of a ultra......-high-resolution line-pair phantome with both systems. Secondly, we investigated 21 healthy volunteers of different phototypes with HD-OCT and RCM on volar forearm and compared the generated images. HD-OCT displays also differences depending on the skin phototype and anatomical site. The 3-μm lateral resolution...... of the HD-OCT could be confirmed by the phantom analysis. The identification of cells in the epidermis can be made by both techniques. RCM offers the best lateral resolution, and HD-OCT has the best penetration depth, providing images of individual cells deeper within the dermis. Eccrine ducts and hair...

  11. Thorium effect on the oxidation of uranium: Photoelectron spectroscopy (XPS/UPS) and cyclic voltammetry (CV) investigation on (U1 − xThx)O2 (x = 0 to 1) thin films

    NARCIS (Netherlands)

    Cakir, P.; Eloirdi, R; Huber, F.; Konings, R.J.M.; Gouder, T

    2017-01-01

    Thin films of U1− xThxO2 (x = 0 to 1) have been deposited via reactive DC sputter technique and characterized by X-ray/Ultra-violet Photoelectron Spectroscopy (XPS/UPS), X-ray Powder Diffractometer (XRD) and Cyclic Voltammetry (CV) in order to understand the

  12. A perspective on two chemometrics tools: PCA and MCR, and introduction of a new one: Pattern recognition entropy (PRE), as applied to XPS and ToF-SIMS depth profiles of organic and inorganic materials

    Science.gov (United States)

    Chatterjee, Shiladitya; Singh, Bhupinder; Diwan, Anubhav; Lee, Zheng Rong; Engelhard, Mark H.; Terry, Jeff; Tolley, H. Dennis; Gallagher, Neal B.; Linford, Matthew R.

    2018-03-01

    X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) are much used analytical techniques that provide information about the outermost atomic and molecular layers of materials. In this work, we discuss the application of multivariate spectral techniques, including principal component analysis (PCA) and multivariate curve resolution (MCR), to the analysis of XPS and ToF-SIMS depth profiles. Multivariate analyses often provide insight into data sets that is not easily obtained in a univariate fashion. Pattern recognition entropy (PRE), which has its roots in Shannon's information theory, is also introduced. This approach is not the same as the mutual information/entropy approaches sometimes used in data processing. A discussion of the theory of each technique is presented. PCA, MCR, and PRE are applied to four different data sets obtained from: a ToF-SIMS depth profile through ca. 100 nm of plasma polymerized C3F6 on Si, a ToF-SIMS depth profile through ca. 100 nm of plasma polymerized PNIPAM (poly (N-isopropylacrylamide)) on Si, an XPS depth profile through a film of SiO2 on Si, and an XPS depth profile through a film of Ta2O5 on Ta. PCA, MCR, and PRE reveal the presence of interfaces in the films, and often indicate that the first few scans in the depth profiles are different from those that follow. PRE and backward difference PRE provide this information in a straightforward fashion. Rises in the PRE signals at interfaces suggest greater complexity to the corresponding spectra. Results from PCA, especially for the higher principal components, were sometimes difficult to understand. MCR analyses were generally more interpretable.

  13. XPS study of influence of exposure to air on thermal stability and kinetics of hydrogen decomposition of MgH{sub 2} films obtained by direct hydrogenation from gaseous phase of metallic Mg

    Energy Technology Data Exchange (ETDEWEB)

    Dobrovolsky, V.D., E-mail: dobersh@ipms.kiev.ua; Khyzhun, O.Y.; Sinelnichenko, A.K.; Ershova, O.G.; Solonin, Y.M.

    2017-02-15

    Highlights: • Air influence on thermal stability of MgH{sub 2} have been studied by XPS. • XPS spectra of MgH{sub 2} films obtained at different hydrogen pressures have been studied. • Changes in the chemical state of MgH{sub 2} films depending on time of exposure to air are analyzed. • Correlation exists between chemical surface condition of MgH{sub 2} films and their thermal stableness. • Process of hydrogen desorption from MgH{sub 2} films is studied using TDS for model samples. - Abstract: Mechanism of influence of exposure to air on thermal stability of MgH{sub 2} obtained by direct hydrogenation from the gas phase, the nature of the hydride sensitivity to the negative impact of air and the role of its surface chemical state have not been studied enough. The present article presents data of X-ray photoelectron spectroscopy (XPS) measurements of the Mg 2s, O 1s, C 1s core-level spectra of surface of hydride MgH{sub 2} films derived by gas phase hydrogenation of model samples of metallic Mg, and the evolution of changes in the chemical state of the surface of the hydride films depending on the time of exposure to air and formation conditions (hydrogen pressure and hydrogenation regime). Based on results of XPS, X-ray diffraction (XRD), and thermodesorption spectroscopy (TDS), the existence of a relationship (correlation) between chemical surface condition of hydride MgH{sub 2} films obtained at different hydrogen pressures (3.0 MPa and 11.5 MPa) and their thermal stableness and temperature of the beginning of hydride decomposition has been established.

  14. Synchrotron-based XPS studies of AlGaN and GaN surface chemistry and its relationship to ion sensor behaviour

    Energy Technology Data Exchange (ETDEWEB)

    Khir, Farah Liyana Muhammad, E-mail: 21001899@student.uwa.edu.au [School of Electrical, Electronic and Computer Engineering, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia); Myers, Matthew, E-mail: Matt.Myers@csiro.au [School of Chemistry and Biochemistry, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia); CSIRO Earth Science and Resource Engineering, Kensington, Western Australia 6151 (Australia); Podolska, Anna [School of Electrical, Electronic and Computer Engineering, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia); Department of Exploration Geophysics, Curtin University of Technology, 26 Dick Perry Avenue, ARRC, Kensington, Western Australia 6151 (Australia); Sanders, Tarun Maruthi [School of Electrical, Electronic and Computer Engineering, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia); Baker, Murray V., E-mail: murray.baker@uwa.edu.au [School of Chemistry and Biochemistry, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia); Nener, Brett D., E-mail: brett.nener@uwa.edu.au [School of Electrical, Electronic and Computer Engineering, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia); Parish, Giacinta, E-mail: giacinta.parish@uwa.edu.au [School of Electrical, Electronic and Computer Engineering, The University of Western Australia, 35 Stirling Hwy., Crawley, Western Australia 6009 (Australia)

    2014-09-30

    Highlights: • Soft X-ray was used to study the surface chemistry of GaN and AlGaN. • The surface chemistry and sensor behaviour were investigated. • The oxide of aluminum is significantly more reactive than gallium. • The Cl{sup −} ions are greater in GaN samples compared to AlGaN samples. - Abstract: Soft X-ray photoelectron spectroscopy was used to investigate the fundamental surface chemistry of both AlGaN and GaN surfaces in the context of understanding the behaviour of AlGaN/GaN heterostructures as chemical field-effect transistor (CHEMFET) ion sensors. AlGaN and GaN samples were subjected to different methods of oxide growth (native oxide and thermally grown oxide) and chemical treatment conditions. Our investigations indicate that the etching of the oxide layer is more pronounced with AlGaN compared to GaN. Also, we observed that chloride ions have a greater tendency to attach to the GaN surface relative to the AlGaN surface. Furthermore, chloride ions are comparatively more prevalent on surfaces treated with 5% HCl acid solution. The concentration of chloride ions is even higher on the HCl treated native oxide surface resulting in a very clear deconvolution of the Cl 2p{sub 1/2} and Cl 2p{sub 3/2} peaks. For GaN and AlGaN surfaces, a linear response (e.g. source-drain current) is typically seen with variation in pH of buffered solutions with constant reference electrode voltage at the surface gate; however, an inverted bath-tub type response (e.g. a maximum at neutral pH and lower values at pH values away from neutral) and a general tendency to negative charge selectivity has been also widely reported. We have shown that our XPS investigations are consistent with the different sensor response reported in the literature for these CHEMFET devices and may help to explain the differing response of these materials.

  15. Characterisation of Pb(Mn{sub 1/3}Nb{sub 2/3})O{sub 3} ceramics by SEM, XRD, XPS and dielectric permittivity tests

    Energy Technology Data Exchange (ETDEWEB)

    Molak, A. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland)]. E-mail: molak@us.edu.pl; Talik, E. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Kruczek, M. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Paluch, M. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Ratuszna, A. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Ujma, Z. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland)

    2006-03-15

    The Pb(Mn{sub 1/3}Nb{sub 2/3})O{sub 3} ceramics has been obtained from oxides by sintering in air, using a two-stage process with precursor columbite-like (Mn{sub 0.5}Nb)O{sub 3} phase. The PbO oxide was added in the second stage. Analysis of the X-ray diffraction pattern shows that the ceramics consist of 91% of major perovskite phase. A monoclinic distortion of the perovskite structure was found. The cell parameters are a = 12.193(3) A, b = 11.966(6) A, c 12.144(2) A, {beta} = 90{sup o}10.7'. The microanalysis made with SEM exhibited fluctuation in chemical composition of the perovskite phase. Precipitation of MnO{sub 2}, PbO and the Pb-Mn-Nb-O phase different from perovskite was found. The X-ray photoelectron spectroscopy was used to study the electronic structure of the Pb(Mn{sub 1/3}Nb{sub 2/3})O{sub 3} ceramics. The core levels of lead, manganese, niobium and oxygen were measured. The shape of valence band ridge is influenced by Mn 3d states. The real average chemical composition obtained from the XPS measurement is Pb{sub 0.99}(Mn{sub 0.42}Nb{sub 0.67})O{sub 2.92}. Broadband dielectric measurement was carried out in 10{sup -2} to 10{sup 6} Hz and within 80-700 K ranges. The dominant relaxation process exhibits characteristic times typical for ionic processes {tau} {sub 0,H} = 1 x 10{sup -11} s for the higher temperature range and, {tau} {sub 0,L} = 1 x 10{sup -9} s for lower temperatures. The activation energy of relaxation process, E {sub M,H} = 0.43 eV and E {sub M,L} = 0.34 eV corresponds to activation energy of electric conductivity. The dielectric relaxation is ascribed to dipoles created by oxygen vacancies and/or Mn-V {sub O} complexes.

  16. Characterization of the surface film on Zr-based bulk metallic glass using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM)

    International Nuclear Information System (INIS)

    Tan Ming; Liu Qiao; Zhang Nian; Hu Huiqin; Li Biao; Kang Xianjie

    2011-01-01

    Highlights: → In this study, we have made four interesting observations. → First, the composition of Al metal ions in the film of the as-cast metallic glass (41%) is much higher than the nominal Al composition of the alloy (9.5%). → We suggest that this should be attributed to the preferential oxidation of Al atoms. → Second, the composition of Al ions in the film of the immersed metallic glass decreases significantly, indicating that the toxic Al oxide and Al ions in the film are dissolved into the solutions during immersion. → Third, the concentration of Cl - ions has no significant effect on the compositions of metal ions in the film. → Fourth, the composition of Zr ions dominates in the film of the immersed metallic glass, indicating that the ZrO 2 oxide in the film is very hard to get corroded in the corrosive solutions. - Abstract: Using XPS, we have for the first time studied the release of metal ions in the film of the Zr-based bulk metallic glass to the corrosive solutions during immersing. The composition of Al ions in the film of the as-cast metallic glass (41%) is substantially higher than the nominal Al composition of the alloy (9.5%). We proposed that the enriched Al ions can be attributed to the preferential oxidation of Al atoms. After immersing in the NaCl- and HCl-solution, the composition of Al ions in the films decreases from 41% to 28.09% and 21.76%, respectively. This indicates that some of the Al ions in the film are dissolved into the solution during immersion. The composition changes of metal ions in the film of the immersed alloys relative to those of the as-cast metallic glass were discussed using the point defect model. SEM was also used to examine the surface morphology of the samples. No pit corrosion was observed in the SEM images of the immersed metal glass.

  17. XPS study of Li/Nb ratio in LiNbO{sub 3} crystals. Effect of polarity and mechanical processing on LiNbO{sub 3} surface chemical composition

    Energy Technology Data Exchange (ETDEWEB)

    Skryleva, E.A., E-mail: easkryleva@gmail.com; Kubasov, I.V., E-mail: kubasov.ilya@gmail.com; Kiryukhantsev-Korneev, Ph.V., E-mail: kiruhancev-korneev@yandex.ru; Senatulin, B.R., E-mail: borisrs@yandex.ru; Zhukov, R.N., E-mail: rom_zhuk@mail.ru; Zakutailov, K.V., E-mail: zakkonst@gmail.com; Malinkovich, M.D., E-mail: malinkovich@yandex.ru; Parkhomenko, Yu.N., E-mail: parkh@rambler.ru

    2016-12-15

    Highlights: • XPS Li/Nb ratio measurement uncertainty in LNbO3 specimens was obtained. • The effect of polarization on surface chemistry was observed only on cleaves. • Li/Nb ratio on positive cleave surface is higher than on negative one. • The positive cleave surface adsorbs fluorine more efficiently than negative one. • Mechanical processing of crystals reduces surface Li/Nb. - Abstract: Different sections of congruent lithium niobate (CLN) crystals have been studied using X-ray photoelectron spectroscopy (XPS). We have developed a method for measuring the lithium-to-niobium atomic ratio Li/Nb from the ratio of the Li1s and Nb4s spectral integral intensities with an overall error of within 8 %. Polarity and mechanical processing affect the Li/Nb ratio on CLN crystal surfaces. The Li/Nb ratio is within the tolerance (0.946 ± 0.074) on the negative cleave surface Z, and there is excess lithium (Li/Nb = 1.25 ± 0.10) on the positive surface. The positive surfaces of the 128° Y cut plates after long exposure to air exhibit LiOH formation indications (obvious lithium excess, higher Li1s spectral binding energy and a wide additional peak in the O1s spectrum produced by nonstructural oxygen). XPS and glow discharge optical electron spectroscopy showed that mechanical processing of differently oriented crystals (X, Z and 128° Y) and different polarities dramatically reduces the Li/Nb ratio. In situ fluorine adsorption experiments revealed the following regularities: fluorine adsorption only occurred on crystal cleaves and was not observed for mechanically processed specimens. Positive cleave surfaces have substantially higher fluorine adsorption capacity compared to negative ones.

  18. Thorium effect on the oxidation of uranium: Photoelectron spectroscopy (XPS/UPS) and cyclic voltammetry (CV) investigation on (U{sub 1−x}Th{sub x})O{sub 2} (x = 0 to 1) thin films

    Energy Technology Data Exchange (ETDEWEB)

    Cakir, P., E-mail: pelincakir@outlook.com [European Commission, Joint Research Centre, P.O. Box 2340, D-76125, Karlsruhe (Germany); Department of Radiation Science and Technology, Delft University of Technology, Mekelweg 15, 2629, JB Delft (Netherlands); Eloirdi, R.; Huber, F. [European Commission, Joint Research Centre, P.O. Box 2340, D-76125, Karlsruhe (Germany); Konings, R.J.M. [European Commission, Joint Research Centre, P.O. Box 2340, D-76125, Karlsruhe (Germany); Department of Radiation Science and Technology, Delft University of Technology, Mekelweg 15, 2629, JB Delft (Netherlands); Gouder, T. [European Commission, Joint Research Centre, P.O. Box 2340, D-76125, Karlsruhe (Germany)

    2017-01-30

    Highlights: • XRD and XPS data of U{sub x}Th{sub 1-x}O{sub 2} films are in agreement with data obtained on bulk. • Oxygen affinity of thorium is much stronger than uranium. • Oxidation of uranium decreases as a function of thorium in the matrix. • XPS made pre and post CV shows thorium enrichment indicating a protective layer. • Higher initial uranium content is directly proportional to higher oxidation states. - Abstract: Thin films of U{sub 1−x}Th{sub x}O{sub 2} (x = 0 to 1) have been deposited via reactive DC sputter technique and characterized by X-ray/Ultra-violet Photoelectron Spectroscopy (XPS/UPS), X-ray Powder Diffractometer (XRD) and Cyclic Voltammetry (CV) in order to understand the effect of Thorium on the oxidation mechanism. During the deposition, the competition between uranium and thorium for oxidation showed that thorium has a much higher affinity for oxygen. Deposition conditions, time and temperature were also the subject of this study, to look at the homogeneity and the stability of the films. While core level and valence band spectra were not altered by the time of deposition, temperature was affecting the oxidation state of uranium and the valence band due to the mobility increase of oxygen through the film. X-ray diffraction patterns, core level spectra obtained for U{sub 1−x}Th{sub x}O{sub 2} versus the composition showed that lattice parameters follow the Vegard's law and together with the binding energies of U-4f and Th-4f are in good agreement with literature data obtained on bulk compounds. To study the effect of thorium on the oxidation of U{sub 1−x}Th{sub x}O{sub 2} films, we used CV experiments at neutral pH of a NaCl solution in contact with air. The results indicated that thorium has an effect on the uranium oxidation as demonstrated by the decrease of the current of the oxidation peak of uranium. XPS measurements made before and after the CV, showed a relative enrichment of thorium at the extent of uranium at

  19. An in situ XPS study of growth of ITO on amorphous hydrogenated Si: Initial stages of heterojunction formation upon processing of ITO/a-Si:H based solar cell structures

    Energy Technology Data Exchange (ETDEWEB)

    Diplas, Spyros; Thoegersen, Annett; Ulyashin, Alexander [SINTEF Materials and Chemistry, Oslo (Norway); Romanyuk, Andriy [University of Basel, Basel (Switzerland)

    2015-01-01

    In this work we studied the interface growth upon deposition of indium-tin oxide (ITO) on amorphous hydrogenated Si (a-Si:H)/crystalline Si (c-Si) structures. The analysis methods used were X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS) in combination with in situ film growth with magnetron sputtering. The analysis was complemented with transmission electron microscopy (TEM) of the deposited films. The sputtering equipment was attached to the XPS spectrometer and hence early stage film growth was observed without breaking the vacuum. It was shown that during early deposition stages ITO is reduced by a-Si:H. The reduction is accompanied with formation of metallic In and Sn at the interface. Formation of Sn is more enhanced on a-Si substrates whilst formation of In is more dominant on c-Si substrates. The reduction effect is less intense for amorphous hydrogenated Si as compared to crystalline Si and this is attributed to stronger presence of dangling bonds in the latter than the former. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  20. Combined atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and quartz crystal microbalance (QCM) studies of glucose oxidase (GOx) immobilised onto self-assembled monolayer on the gold film

    International Nuclear Information System (INIS)

    Losic, D.; Shapter, J.; Gooding, J.; Erokin, P.; Short, K.

    1999-01-01

    In fabrication of biosensors, self-assembled monolayers (SAM) are an attractive method of immobilising enzymes at electrode surface since it allows precise control over the amount and spatial distribution of the immobilized enzyme. The covalent attachment of glucose oxidase (GOx) to a carboxylic terminated SAM chemisorbed onto gold films was achieved via carbodiimide activation of the carboxylic acids to a reactive intermediate susceptible to nucleophilic attack by amines on free lysine chains of the enzyme. Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and quartz crystal microbalance (QCM) measurements were used for characterisation of GOx modified gold surfaces. Tapping mode AFM studies have revealed that GOx molecules form slightly disordered arrays of pentagonal or hexagonal clusters. Observed features of immobilised GOx are distributed as a submonolayer on the SAM surface which has allowed visualisation of native and unfolded enzyme structure. The presence of the SAM and enzyme on the gold surface was detected by XPS spectroscopy. Spectra show typical peaks for the C 1s, O 1s and N 1s regions. A kinetic study of the adsorption of GOx onto activated SAM using in-situ QCM allowed determination the amount of immobilised GOx on the layer and consequently the optimal immobilisation conditions. Performance parameters of the biosensor such as sensitivity to glucose concentration as a function of enzyme loading were evaluated amperometrically using the redox mediator p-benzoquinone

  1. XPS-UPS, ISS characterization studies and the effect of Pt and K addition on the catalytic properties of MoO2-x(OH)y deposited on TiO2

    International Nuclear Information System (INIS)

    Al-Kandari, H.; Mohamed, A.M.; Al-Kharafi, F.; Katrib, A.

    2011-01-01

    Highlights: → Surface electronic structure-catalytic activity correlation is presented in this research work. → In situ characterization by XPS-UPS and ISS techniques were employed at the same experimental conditions applied for catalytic reactions. → Catalytic reactions of Mo deposited on titanium oxide for the isomerization and hydrogenation reactions using 1-hexene and n-hexane were studied. → The bifunctional properties of the molybdenum dioxide phase were modified by the addition of potassium. - Abstract: Characterization by XPS-UPS, ISS surface techniques of MoO 3 /TiO 2 catalysts before and after addition of Pt (PtMo) 2.5% by weight of MoO 3 and potassium (KMo) enabled to identify different chemical species present on the outermost surface layer at different reduction temperatures. Catalytic activities of these systems using 1-hexene and n-hexane reactants were studied. Correlation between catalytic activity and surface electronic structure enabled us to identify the chemical species, active site(s), responsible for specific catalytic reaction(s).

  2. XPS-UPS, ISS characterization studies and the effect of Pt and K addition on the catalytic properties of MoO{sub 2-x}(OH){sub y} deposited on TiO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Al-Kandari, H. [Public Authority of Applied Education and Training (Kuwait); Mohamed, A.M.; Al-Kharafi, F. [Kuwait University, Department of Chemistry, P.O. Box 5969, Safat 13060 (Kuwait); Katrib, A., E-mail: ali.katrib@ku.edu.kw [Kuwait University, Department of Chemistry, P.O. Box 5969, Safat 13060 (Kuwait)

    2011-11-15

    Highlights: {yields} Surface electronic structure-catalytic activity correlation is presented in this research work. {yields} In situ characterization by XPS-UPS and ISS techniques were employed at the same experimental conditions applied for catalytic reactions. {yields} Catalytic reactions of Mo deposited on titanium oxide for the isomerization and hydrogenation reactions using 1-hexene and n-hexane were studied. {yields} The bifunctional properties of the molybdenum dioxide phase were modified by the addition of potassium. - Abstract: Characterization by XPS-UPS, ISS surface techniques of MoO{sub 3}/TiO{sub 2} catalysts before and after addition of Pt (PtMo) 2.5% by weight of MoO{sub 3} and potassium (KMo) enabled to identify different chemical species present on the outermost surface layer at different reduction temperatures. Catalytic activities of these systems using 1-hexene and n-hexane reactants were studied. Correlation between catalytic activity and surface electronic structure enabled us to identify the chemical species, active site(s), responsible for specific catalytic reaction(s).

  3. Lateral resolution of desorption nanoelectrospray: a nanospray tip without nebulizing gas as a source of primary charged droplets

    Czech Academy of Sciences Publication Activity Database

    Hartmanová, L.; Lorencová, I.; Volný, M.; Fryčák, P.; Havlíček, Vladimír; Chmelíčková, Hana; Ingr, T.; Lemr, K.

    2016-01-01

    Roč. 141, č. 7 (2016), s. 2150-2154 ISSN 0003-2654 R&D Projects: GA ČR(CZ) GAP206/12/1150 Institutional support: RVO:61388971 ; RVO:68378271 Keywords : IONIZATION MASS-SPECTROMETRY * ELECTROSPRAY-IONIZATION * AMBIENT CONDITIONS Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 3.885, year: 2016

  4. Thermogravimetric analysis, PXRD, EDX and XPS study of chrysocolla (Cu,Al)2H2Si2O5(OH)4·nH2O-structural implications

    International Nuclear Information System (INIS)

    Frost, Ray L.; Xi, Yunfei; Wood, Barry J.

    2012-01-01

    Highlights: ► We have undertaken a TG X PS study of the mineral chrysocolla. ► The chemical bonding of Cu, O and Si has been determined. ► It is concluded that chrysocolla is a mineral in its own right. ► It is not a colloidal mixture of spertiniite and amorphous silica. - Abstract: Selected chrysocolla mineral samples from different origins have been studied by using PXRD, SEM, EDX and XPS. The XRD patterns show that the chrysocolla mineral samples are non-diffracting and no other phases are present in the minerals, thus showing the chrysocolla samples are pure. SEM analyses show the chrysocolla surfaces are featureless. EDX analyses enable the formulae of the chrysocolla samples to be calculated. The thermal decomposition of the mineral chrysocolla has been studied using a combination of thermogravimetric analysis and derivative thermogravimetric analysis. Five thermal decomposition mass loss steps are observed for the chrysocolla from Arizona (a) at 125 °C with the loss of water, (b) at 340 °C with the loss of hydroxyl units, (c) at 468.5 °C with a further loss of hydroxyls, (d) at 821 °C with oxygen loss and (e) at 895 °C with a further loss of oxygen. The thermal analysis of the chrysocolla from Congo shows mass losses at 125, 275.3, 805.6 and 877.4 °C and for the Nevada chrysocolla, mass loss steps at 268, 333, 463, 786.0 and 817.7 °C are observed. The thermal analysis of spertiniite is very different from that of chrysocolla and thermally decomposes at around 160 °C. XPS shows that there are two different copper species present, one which is bonded to oxygen and one to a hydroxyl unit. The O 1s is broad and very symmetrical suggesting two O species of equal number. The bond energy of 102.9 eV for the Si 2p suggests that it is in the form of a silicate. The bond energy is much higher for silicas around ∼103.5 eV. The reported value for silica gel has Si 2p at 103.4 eV. The combination of TG, PXRD, EDX and XPS adds to our fundamental

  5. Quantitative assessment of rat corneal thickness and morphology during stem cell therapy by high-speed optical coherence tomography

    Science.gov (United States)

    Lal, Cerine; McGrath, James; Subhash, Hrebesh; Rani, Sweta; Ritter, Thomas; Leahy, Martin

    2016-03-01

    Optical Coherence Tomography (OCT) is a non-invasive 3 dimensional optical imaging modality that enables high resolution cross sectional imaging in biological tissues and materials. Its high axial and lateral resolution combined with high sensitivity, imaging depth and wide field of view makes it suitable for wide variety of high resolution medical imaging applications at clinically relevant speed. With the advent of swept source lasers, the imaging speed of OCT has increased considerably in recent years. OCT has been used in ophthalmology to study dynamic changes occurring in the cornea and iris, thereby providing physiological and pathological changes that occur within the anterior segment structures such as in glaucoma, during refractive surgery, lamellar keratoplasty and corneal diseases. In this study, we assess the changes in corneal thickness in the anterior segment of the eye during wound healing process in a rat corneal burn model following stem cell therapy using high speed swept source OCT.

  6. Fischer-Tropsch synthesis: study of the promotion of Pt on the reduction property of Co/Al2O3 catalysts by in situ EXAFS of Co K and Pt LIII edges and XPS

    International Nuclear Information System (INIS)

    Jacobs, G.; Chaney, J.A.; Patterson, P.M.; Das, T.K.; Maillot, J.C.; Davis, B.H.

    2004-01-01

    The addition of platinum metal to cobalt/alumina-based Fischer-Tropsch synthesis (FTS) catalysts increases both the reduction rate and, consequently, the density of active cobalt sites. Platinum also lowers the temperature of the two-step conversion of cobalt oxide to cobalt metal observed in temperature programmed reduction (TPR) as Co 3 O 4 to CoO and CoO to Co 0 . The interaction of the alumina support with cobalt oxide ultimately determines the active site density of the catalyst surface. This interaction can be controlled by varying the cobalt loading and dispersion, selecting supports with differing surface areas or pore sizes, or changing the noble metal promoter. However, the active site density is observed to depend primarily on the cluster size and extent of reduction, and there is a direct relationship between site density and FTS rate. In this work, in situ extended X-ray absorption fine structure (EXAFS) at the L III edge of Pt was used to show that isolated Pt atoms interact with supported cobalt clusters without forming observable Pt-Pt bonds. K-edge EXAFS was also used to verify that the cobalt cluster size increases slightly for those systems with Pt promotion. X-ray absorption near-edge spectroscopy (XANES) was used to examine the remaining cobalt clusters after the first stage of TPR, and it revealed that the species were almost entirely cobalt (II) oxide. After the second stage of TPR to form cobalt metal, a residual oxide persists in the sample, and this oxide has been identified as cobalt (II) aluminate using X-ray photoelectron spectroscopy (XPS). Sequential in situ reduction of promoted and unpromoted systems was also monitored through XPS, and Pt was seen to increase the extent of cobalt reduction by a factor of two. (orig.)

  7. High-resolution high-sensitivity elemental imaging by secondary ion mass spectrometry: from traditional 2D and 3D imaging to correlative microscopy

    International Nuclear Information System (INIS)

    Wirtz, T; Philipp, P; Audinot, J-N; Dowsett, D; Eswara, S

    2015-01-01

    Secondary ion mass spectrometry (SIMS) constitutes an extremely sensitive technique for imaging surfaces in 2D and 3D. Apart from its excellent sensitivity and high lateral resolution (50 nm on state-of-the-art SIMS instruments), advantages of SIMS include high dynamic range and the ability to differentiate between isotopes. This paper first reviews the underlying principles of SIMS as well as the performance and applications of 2D and 3D SIMS elemental imaging. The prospects for further improving the capabilities of SIMS imaging are discussed. The lateral resolution in SIMS imaging when using the microprobe mode is limited by (i) the ion probe size, which is dependent on the brightness of the primary ion source, the quality of the optics of the primary ion column and the electric fields in the near sample region used to extract secondary ions; (ii) the sensitivity of the analysis as a reasonable secondary ion signal, which must be detected from very tiny voxel sizes and thus from a very limited number of sputtered atoms; and (iii) the physical dimensions of the collision cascade determining the origin of the sputtered ions with respect to the impact site of the incident primary ion probe. One interesting prospect is the use of SIMS-based correlative microscopy. In this approach SIMS is combined with various high-resolution microscopy techniques, so that elemental/chemical information at the highest sensitivity can be obtained with SIMS, while excellent spatial resolution is provided by overlaying the SIMS images with high-resolution images obtained by these microscopy techniques. Examples of this approach are given by presenting in situ combinations of SIMS with transmission electron microscopy (TEM), helium ion microscopy (HIM) and scanning probe microscopy (SPM). (paper)

  8. High resolution X-ray photoelectron spectroscopy of styrene oxide adsorption and reaction on Ag(1 1 1)

    Science.gov (United States)

    Piao, H.; Enever, M. C. N.; Adib, K.; Hrbek, J.; Barteau, M. A.

    2004-11-01

    Synchrotron-based X-ray photoelectron spectroscopy (XPS) has been used to investigate the adsorption and reaction of styrene oxide on Ag(1 1 1). When adsorption is carried out at 250 K or above, ring opening of styrene oxide forms a stable surface oxametallacycle intermediate which eventually reacts at 485 K to regenerate styrene oxide. High resolution XPS is capable of distinguishing the oxametallacycle from molecularly adsorbed and condensed styrene oxide on the basis of different C1s peak separations. The observed separations are well accounted for by the results of DFT calculations.

  9. XPS and SEM analysis of the surface of gas atomized powder precursor of ODS ferritic steels obtained through the STARS route

    Science.gov (United States)

    Gil, E.; Cortés, J.; Iturriza, I.; Ordás, N.

    2018-01-01

    An innovative powder metallurgy route to produce ODS FS, named STARS, has succeeded in atomizing steel powders containing the oxide formers (Y and Ti) and, hence, avoids the mechanical alloying (MA) step to dissolve Y in the matrix. A metastable oxide layer forms at the surface of atomized powders and dissociates during HIP consolidation at high temperatures, leading to precipitation of more stable Y-Ti-O nanoparticles.

  10. A Reactive Oxide Overlayer on Rh Nanoparticles during CO Oxidation and Its Size Dependence Studied by in Situ Ambient Pressure XPS

    International Nuclear Information System (INIS)

    Grass, Michael E.; Zhang, Yawen; Butcher, Derek R.; Park, Jeong Y.; Li, Yimin; Bluhm, Hendrik; Bratlie, Kaitlin M.; Zhang, Tianfu; Somorjai, Gabor A.

    2008-01-01

    CO oxidation is one of the most studied heterogeneous reactions, being scientifically and industrially important, particularly for removal of CO from exhaust streams and preferential oxidation for hydrogen purification in fuel cell applications. The precious metals Ru, Rh, Pd, Pt, and Au are most commonly used for this reaction because of their high activity and stability. Despite the wealth of experimental and theoretical data, it remains unclear what is the active surface for CO oxidation under catalytic conditions for these metals. In this communication, we utilize in situ synchrotron ambient pressure X-ray photoelectron spectroscopy (APXPS) to monitor the oxidation state at the surface of Rh nanoparticles during CO oxidation and demonstrate that the active catalyst is a surface oxide, the formation of which is dependent on particle size. The amount of oxide formed and the reaction rate both increase with decreasing particle size.

  11. Microstructural, Raman and XPS properties of single-crystalline Bi3.15Nd0.85Ti3O12 nanorods

    International Nuclear Information System (INIS)

    Hu Zhenglong; Gu Haoshuang; Hu Yongming; Zou Yanan; Zhou Di

    2009-01-01

    Bi 3.15 Nd 0.85 Ti 3 O 12 (BNT) nanorods were successfully synthesized first time by hydrothermal method. The nanorods are uniform along their length, and are composed of single-crystalline BNT with orthorhombic structure. The diameters of BNT nanorods are about 30-120 nm and growth along the [1 0 4] direction, which are promising candidate for nanoscale ferroelectric sensors. Ten Raman active modes were observed for orthorhombic phase BNT nanorods, which are overdamped and highly shifted compare to that of Bi 4 Ti 3 O 12 (BIT) powders. The chemical composition of the samples and the valence states of elements were determined by X-ray photoelectron spectroscopy

  12. Solar2Fuel: XPS and TPD characterization of functionalized TiO{sub 2} surfaces for photocatalytic reduction of CO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Staier, Florian; Grunze, Michael; Zharnikov, Michael [Angewandte Physikalische Chemie, Universitaet Heidelberg, INF 253, 69120 Heidelberg (Germany)

    2011-07-01

    The handling of CO{sub 2} produced by industrial installations and power plants has become a very important environmental issue nowadays because of it's generally accepted impact on the green house effect. In this context, a storage of CO{sub 2} or its conversation to fuel or useful chemicals are highly desirable. Along these lines, the solar2fuel project, funded by BMBF, aims on photocatalytic conversion of CO{sub 2} to methanol with a sufficient quantum efficiency which can justify and make rentable an industrial realization of the process. As the primary catalytic system TiO{sub 2} nanoparticle powder coatings are used. These particles are doped with metals to enhance their catalytic activity and functionalized with specially designed dyes which promote photocatalytic reaction and move the absorption spectrum from UV (characteristic of TiO{sub 2}) to the visible range. We present first results on characterization of these catalytic systems by several complimentary techniques as well as on temperature-programmed-desorption of CO{sub 2} and methanol from these functionalized surfaces.

  13. Soft electronic structure modulation of surface (thin-film) and bulk (ceramics) morphologies of TiO{sub 2}-host by Pb-implantation: XPS-and-DFT characterization

    Energy Technology Data Exchange (ETDEWEB)

    Zatsepin, D.A. [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, 620990 Yekaterinburg (Russian Federation); Institute of Physics and Technology, Ural Federal University, 620002 Yekaterinburg (Russian Federation); Boukhvalov, D.W., E-mail: danil@hanyang.ac.kr [Department of Chemistry, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Theoretical Physics and Applied Mathematics Department, Ural Federal University, Mira Street 19, 620002 Yekaterinburg (Russian Federation); Gavrilov, N.V. [Institute of Electrophysics, Russian Academy of Sciences, Ural Branch, 620990 Yekaterinburg (Russian Federation); Zatsepin, A.F. [Institute of Physics and Technology, Ural Federal University, 620002 Yekaterinburg (Russian Federation); Shur, V.Ya.; Esin, A.A. [Institute of Natural Sciences, Ural Federal University, 51 Lenin Ave, 620000 Yekaterinburg (Russian Federation); Kim, S.S. [School of Materials Science and Engineering, Inha University, Incheon 402-751 (Korea, Republic of); Kurmaev, E.Z. [M.N. Miheev Institute of Metal Physics of Ural Branch of Russian Academy of Sciences, 620990 Yekaterinburg (Russian Federation); Institute of Physics and Technology, Ural Federal University, 620002 Yekaterinburg (Russian Federation)

    2017-04-01

    Highlights: • Experiment and theory demonstrate significant difference between patterns of Pb-ion implantation in TiO{sub 2}. • In bulk TiO{sub 2} Pb-impurities leads formation of PbO phase. • On the surface of TiO{sub 2}:Pb occur formation of PbxOy configurations. • In both bulk and surface TiO{sub 2}:Pb occur decreasing of the bandgap by shift of valence band about 1 eV up. - Abstract: The results of combined experimental and theoretical study of substitutional and clustering effects in the structure of Pb-doped TiO{sub 2}-hosts (bulk ceramics and thin-film morphologies) are presented. Pb-doping of the bulk and thin-film titanium dioxide was made with the help of pulsed ion-implantation without posterior tempering (Electronic Structure Modulation Mode). The X-ray photoelectron spectroscopy (XPS) qualification of core-levels and valence bands and Density-Functional Theory (DFT) calculations were employed in order to study the yielded electronic structure of Pb-ion modulated TiO{sub 2} host-matrices. The combined XPS-and-DFT analysis has agreed definitely with the scenario of the implantation stimulated appearance of PbO-like structures in the bulk morphology of TiO{sub 2}:Pb, whereas in thin-film morphology the PbO{sub 2}-like structure becomes dominating, essentially contributing weak O/Pb bonding (Pb{sub x}O{sub y} defect clusters). The crucial role of the oxygen hollow-type vacancies for the process of Pb-impurity “insertion” into the structure of bulk TiO{sub 2} was pointed out employing DFT-based theoretical background. Both experiment and theory established clearly the final electronic structure re-arrangement of the bulk and thin-film morphologies of TiO{sub 2} because of the Pb-modulated deformation and shift of the initial Valence Base-Band Width about 1 eV up.

  14. Spectral artefacts post sputter-etching and how to cope with them - A case study of XPS on nitride-based coatings using monoatomic and cluster ion beams

    Science.gov (United States)

    Lewin, Erik; Counsell, Jonathan; Patscheider, Jörg

    2018-06-01

    The issue of artefacts due to sputter-etching has been investigated for a group of AlN-based thin film materials with varying thermodynamical stability. Stability of the materials was controlled by alloying AlN with the group 14 elements Si, Ge or Sn in two different concentrations. The coatings were sputter-etched with monoatomic Ar+ with energies between 0.2 and 4.0 keV to study the sensitivity of the materials for sputter damage. The use of Arn+ clusters to remove an oxidised surface layer was also evaluated for a selected sample. The spectra were compared to pristine spectra obtained after in-vacuo sample transfer from the synthesis chamber to the analysis instrument. It was found that the all samples were affected by high energy (4 keV) Ar+ ions to varying degrees. The determining factors for the amount of observed damage were found to be the materials' enthalpy of formation, where a threshold value seems to exist at approximately -1.25 eV/atom (∼-120 kJ/mol atoms). For each sample, the observed amount of damage was found to have a linear dependence to the energy deposited by the ion beam per volume removed material. Despite the occurrence of sputter-damage in all samples, etching settings that result in almost artefact-free spectral data were found; using either very low energy (i.e. 200 eV) monoatomic ions, or an appropriate combination of ion cluster size and energy. The present study underlines that analysis post sputter-etching must be carried out with an awareness of possible sputter-induced artefacts.

  15. In vivo high resolution human corneal imaging using full-field optical coherence tomography.

    Science.gov (United States)

    Mazlin, Viacheslav; Xiao, Peng; Dalimier, Eugénie; Grieve, Kate; Irsch, Kristina; Sahel, José-Alain; Fink, Mathias; Boccara, A Claude

    2018-02-01

    We present the first full-field optical coherence tomography (FFOCT) device capable of in vivo imaging of the human cornea. We obtained images of the epithelial structures, Bowman's layer, sub-basal nerve plexus (SNP), anterior and posterior stromal keratocytes, stromal nerves, Descemet's membrane and endothelial cells with visible nuclei. Images were acquired with a high lateral resolution of 1.7 µm and relatively large field-of-view of 1.26 mm x 1.26 mm - a combination, which, to the best of our knowledge, has not been possible with other in vivo human eye imaging methods. The latter together with a contactless operation, make FFOCT a promising candidate for becoming a new tool in ophthalmic diagnostics.

  16. XPS, TEM and NRA investigations of Zn(Se,OH)/Zn(OH){sub 2} films on Cu(In,Ga)(S,Se){sub 2} substrates for highly efficient solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Eisele, W.; Ennaoui, A.; Schubert-Bischoff, P.; Giersig, M.; Pettenkofer, C.; Krauser, J.; Lux-Steiner, M. [Hahn-Meitner Inst., Berlin (Germany); Zweigart, S.; Karg, F. [Siemens and Shell Solar, Munich (Germany)

    2003-01-01

    Structural and compositional properties of Zn(Se,OH)/Zn(OH){sub 2} buffer layers deposited by chemical bath deposition(CBD) on Cu(In,Ga)(S,Se){sub 2} (CIGSS) absorbers are investigated. Due to the aqueous nature of the CBD process, oxygen and hydrogen were incorporated into the 'ZnSe' buffer layer mainly in the form of Zn(OH){sub 2} as is shown by X-ray photoelectron spectroscopy and nuclear reaction analysis (NRA) measurements leading to the nomenclature 'Zn(Se,OH)'. Prior to the deposition of Zn(Se,OH), a zinc treatment of the absorber was performed. During that treatment a layer mainly consisting of Zn(OH){sub 2} grew to a thickness of several nanometer. The whole buffer layer therefore consists of a Zn(Se,OH)/Zn(OH){sub 2} structure on CIGSS. Part of the Zn(OH){sub 2} in both layers (i.e. the Zn(Se,OH) and the Zn(OH){sub 2} layer) might be converted into ZnO during measurements or storage. Scanning electron microscopy pictures showed that a complete coverage of the absorber with the buffer layer was achieved. Transmission electron microscopy revealed the different regions of the buffer layer: An amorphous area (possibly Zn(OH){sub 2}) and a partly nanocrystalline area, where lattice planes of ZnSe could be identified. Solar cell efficiencies of ZnO/Zn(Se,OH)/Zn(OH){sub 2}/CIGSS devices exceed 14% (total area).(author)

  17. YAPI-GNAORE et al..xps

    African Journals Online (AJOL)

    HP Pro 2000

    comparée aux poulets de souche Label Rouge (T55 x SA51) importés de France. Les poulets ... la filière avicole (viande et œufs) parmi les plus prioritaires. .... Tableau 1 : Composition d'aliments de démarrage, de croissance et de finition.

  18. AMARI LDGE et al..xps

    African Journals Online (AJOL)

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    RESPONSE TO JUGLONE TOXIC EFFECT IN VARIOUS. GENOTYPES OF ... Local cultivars and hybrids to ... content of FHIA23 and PITA14 hybrids was at a basal level. These tetraploid ..... measure to an early evaluation of the physiological ...

  19. LEPENGUE AN et al...xps

    African Journals Online (AJOL)

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    Heller R., Esnault R. et C. Lance. 2006. Physiologie végétale. Développement. 6e édition de l'abrégé, Editions Dunod, Paris, 366 p. Lépengué A.N., M'batchi B. et S. Aké. 2007. Impact de Phoma sabdariffae Sacc. sur la croissance et la valeur marchande de la roselle (Hibiscus sabdariffa L. var. sabdariffa) au Gabon. Rev.

  20. NAITORMBAIDE M. et al..xps

    African Journals Online (AJOL)

    HP Pro 2000

    groundnut yield. Phosphate and manure fertilizations were found to be necessary in yield increase. This parameter determines the return on the groundnut. State subventions or easy access to funding can help to disseminate animal drive techniques in order to foster better land management techniques for yield.

  1. First experimental proof for aberration correction in XPEEM: Resolution, transmission enhancement, and limitation by space charge effects

    International Nuclear Information System (INIS)

    Schmidt, Th.; Sala, A.; Marchetto, H.; Umbach, E.; Freund, H.-J.

    2013-01-01

    The positive effect of double aberration correction in x-ray induced Photoelectron Emission Microscopy (XPEEM) has been successfully demonstrated for both, the lateral resolution and the transmission, using the Au 4f XPS peak for element specific imaging at a kinetic energy of 113 eV. The lateral resolution is improved by a factor of four, compared to a non-corrected system, whereas the transmission is enhanced by a factor of 5 at a moderate resolution of 80 nm. With an optimized system setting, a lateral resolution of 18 nm could be achieved, which is up to now the best value reported for energy filtered XPEEM imaging. However, the absolute resolution does not yet reach the theoretical limit of 2 nm, which is due to space charge limitation. This occurs along the entire optical axis up to the contrast aperture. In XPEEM the pulsed time structure of the exciting soft x-ray light source causes a short and highly intense electron pulse, which results in an image blurring. In contrast, the imaging with elastically reflected electrons in the low energy electron microscopy (LEEM) mode yields a resolution clearly below 5 nm. Technical solutions to reduce the space charge effect in an aberration-corrected spectro-microscope are discussed. - Highlights: ► First successful double aberration correction in XPEEM. ► Improvement of resolution and transmission by aberration correction. ► Lateral resolution of 18 nm in energy filtered XPEEM is the best up to now reported value. ► First investigation of space charge effects in aberrations corrected PEEM

  2. Short range structural models of the glass transition temperatures and densities of 0.5Na2S + 0.5[xGeS2 + (1 - x)PS5/2] mixed glass former glasses.

    Science.gov (United States)

    Bischoff, Christian; Schuller, Katherine; Martin, Steve W

    2014-04-03

    The 0.5Na2S + 0.5[xGeS2 + (1 - x)PS5/2] mixed glass former (MGF) glass system exhibits a nonlinear and nonadditive negative change in the Na(+) ion conductivity as one glass former, PS5/2, is exchanged for the other, GeS2. This behavior, known as the mixed glass former effect (MGFE), is also manifest in a negative deviation from the linear interpolation of the glass transition temperatures (T(g)) of the binary end-member glasses, x = 0 and x = 1. Interestingly, the composition dependence of the densities of these ternary MGF glasses reveals a slightly positive MGFE deviation from a linear interpolation of the densities of the binary end-member glasses, x = 0 and x = 1. From our previous studies of the structures of these glasses using IR, Raman, and NMR spectroscopies, we find that a disproportionation reaction occurs between PS7/2(4-) and GeS3(2-) units into PS4(3-) and GeS5/2(1-) units. This disproportionation combined with the formation of Ge4S10(4-) anions from GeS5/2(1-) groups leads to the negative MGFE in T(g). A best-fit model of the T(g)s of these glasses was developed to quantify the amount of GeS5/2(1-) units that form Ge4S10(4-) molecular anions in the ternary glasses (∼ 5-10%). This refined structural model was used to develop a short-range structural model of the molar volumes, which shows that the slight densification of the ternary glasses is due to the improved packing efficiency of the germanium sulfide species.

  3. Chemical degradation of selected Zn-based corrosion products induced by C{sub 60} cluster, Ar cluster and Ar{sup +} ion sputtering in the focus of X-ray photoelectron spectroscopy (XPS)

    Energy Technology Data Exchange (ETDEWEB)

    Steinberger, R., E-mail: roland.steinberger@jku.at [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterization, Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Sicking, J., E-mail: jens.sicking@bayer.com [Bayer AG, Engineering & Technology, Applied Physics, Chempark Building E 41, 51368 Leverkusen (Germany); Weise, J., E-mail: juliane.weise@physik.tu-freiberg.de [Institut für Experimentelle Physik, TU Bergakademie Freiberg, Leipziger Straße 23, 09599 Freiberg (Germany); Duchoslav, J., E-mail: jiri.duchoslav@jku.at [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterization, Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Greunz, T., E-mail: theresia.greunz@jku.at [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterization, Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria); Meyer, D.C., E-mail: Dirk-Carl.Meyer@physik.tu-freiberg.de [Institut für Experimentelle Physik, TU Bergakademie Freiberg, Leipziger Straße 23, 09599 Freiberg (Germany); Stifter, D., E-mail: david.stifter@jku.at [Christian Doppler Laboratory for Microscopic and Spectroscopic Material Characterization, Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz (Austria)

    2017-05-01

    Highlights: • XPS investigations for various sputter concepts on Zn-based corrosions products. • Direct comparison of induced chemical damage for ion and cluster sputtering. • Azimuthal rotation or heavy projectile bombardment was not found to be beneficial. • Ar cluster etching is rated as unsuitable for surface cleaning or depth profiling. • C{sub 60} and Ar{sup +} are applicable for sputtering when degradation is carefully considered. - Abstract: Monoatomic ion sputtering is a common concept for surface sensitive analysis methods to clean surfaces prior investigation or to obtain information from deeper regions. However, severe damage of the materials – linked to preferential sputtering, ion implantation, atomic mixing and in worst case chemical degradation – can affect the validity of the analysis. Hence, the impact of C{sub 60} cluster etching, furthermore, of Ar{sup +} ion bombardment with and without azimuthal sample rotation and also the application of heavy projectiles (Xe{sup +} ions) was investigated to find a concept, which is less destructive or with less critical influence on the chemical nature of the investigated materials. In this work the focus is set on hydrozincite and zinc oxide, two common corrosion products of Zn-based coatings. As a main point, all the obtained results from (i) Ar{sup +} ion, (ii) Ar cluster, and (iii) C{sub 60} cluster etching on the degradation kinetics of hydrozincite were compared with respect to the reached sputter depth. In addition, the sputter rate of all three methods was experimentally determined for ZnO. In total, fully non-destructive conditions could not be found, but valuable knowledge on the type and rate of degradation, which is essential to choose the most suited sputter concept.

  4. AES, EELS and XPS characterization of Ti(C, N, O) films prepared by PLD using a Ti target in N2, CH4, O2 and CO as reactive gases

    International Nuclear Information System (INIS)

    Soto, G.

    2004-01-01

    Titanium-based films were grown on (1 0 0)-Si substrates by the pulsed laser deposition (PLD) method using a Ti target in reactive atmospheres. The films were grown in vacuum (Ti-film), O 2 (TiO x ), N 2 (TiN x ), CH 4 (TiC x ), CO (TiC x O y ), N 2 +CH 4 (TiC x N y ) and CO+N 2 (TiC x N y O z ). After depositions, every film is characterized in situ by Auger, electron-energy loss and X-ray photoelectron (XPS) spectroscopies. For the binary compounds the stoichiometry is regulated without difficulty by gas pressure during ablation. However, for ternary and quaternary compounds there is a tendency to produce chemically inhomogeneous films. For example, the ablation of Ti in a N 2 +CH 4 environment results in a TiNC:C composite. In this case, the overabundance of nitrogen influences the segregation of carbon. In the other hand, the O 2 +CH 4 mixture was ineffectively to produce TiC x O y films, yielding mostly TiO 2 with traces of embedded carbon. By using CO as reactive gas the TiC x O y films were completed. Also, a mixture of CO with N 2 was tested to produce quaternary TiC x N y O z compounds. Based on these results, it is recommended that better control on film stoichiometry and chemical homogeneity can be achieved by using reactive gases with predetermined C:N:O ratios

  5. XPS study of surface state of novel perovskite system Dy{sub 0.5}Sr{sub 0.5}Co{sub 0.8}Fe{sub 0.2}O{sub 3-δ} as cathode for solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Kautkar, Pranay R.; Acharya, Smita A., E-mail: saha275@yahoo.com; Tumram, Priya V. [Depatment of Physics, Rashtrasant Tukadoji Maharaj Nagpur University Campus, Nagpur-440033 (India); Deshpande, U. P. [UGC-DAE Consortium for scientific Research, University Campus, Khandwa Road, Indore-452001, Madhya Pradesh,India (India)

    2016-05-06

    In the present attempt,novel perovskite oxide Dy{sub 0.5}Sr{sub 0.5}Co{sub 0.8}Fe{sub 0.2}O{sub 3–δ} (DSCF) as cathode material has been synthesized by an Ethylene glycol-citrate combined sol-gel combustion route. Orthorhombic symmetry structure is confirmed by X-ray diffraction (XRD) and data is well fitted using Rietveld refinement by Full-Prof software suite. Chemical natureof surface of DSCF has been analyzed by using X-ray photoelectron spectroscopy (XPS). XPS result shows that Dy ions are in +3 oxidation state and Sr in +2 states. However Co2p and Fe2p spectra indicates partial change in oxidation state from Co3+/Fe3+ to Co4+/Fe4+. These attribute to develop active sites on the surface for oxygen ions. O1s XPS spectra shows two oxygen peaks relatedto lattice oxygen in perovskite and absorbed oxygen in oxygen vacancy are detected. O1s spectra demonstrate the existence of adsorbed oxygen species on the surface of DSCF oxide which is quite beneficial for intermediate temperature of Solid Oxide Fuel Cell.

  6. The formation and structure of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 6.4}: XRD Rietveld, Mössabuer and XPS analyses

    Energy Technology Data Exchange (ETDEWEB)

    Al-Rawas, A.D., E-mail: arawas@squ.edu.om [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman); Widatallah, H.M.; Al-Harthi, S.H. [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman); Johnson, C. [Chemistry Department, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Gismelseed, A.M.; Elzain, M.E.; Yousif, A.A. [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman)

    2015-05-15

    Highlights: • The formation of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} is investigated. • Pre-milling the reactants substantially lowers the formation temperature. • The core and surface structures were studied. • XRD and {sup 57}Fe Mössbauer spectroscopic analyses indicate the δ-value to be 0.60. • XPS shows a complex surface structure for the mechanosynthesized Sr{sub 3}Fe{sub 2}O{sub 7−δ} nanoparticles. - Abstract: The influence of ball milling and subsequent sintering of a 3:1 molar mixture of SrCO{sub 3} and α-Fe{sub 2}O{sub 3} on the formation of Sr{sub 3}Fe{sub 2}O{sub 7−δ} double perovskite is investigated with different analytical techniques. Milling the mixture for 110 h leads to the formation of SrCO{sub 3}-α-Fe{sub 2}O{sub 3} nanocomposites and the structural deformation of α-Fe{sub 2}O{sub 3} via the incorporation of Sr{sup 2+} ions. Subsequent sintering of the pre-milled reactants’ mixture has led to the partial formation of an SrFeO{sub 3} perovskite-related phase in the temperature range 400–600 °C. This was followed by the progressive development of an Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase that continued to increase with increasing sintering temperature until a single-phased nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase was attained at 950 °C (12 h). This temperature is ∼350 °C lower than the temperature at which the material is prepared conventionally using the ceramic method. The evolution of different structural phases during the reaction process is discussed. Rietveld refinement of the X-ray diffraction data shows a value of 0.60 for the oxygen deficiency δ, in consistency with the Fe{sup 3+}/Fe{sup 4+} ratio derived from the {sup 57}Fe Mössbauer data recorded at both 300 K and 78 K. The Mössbauer data suggests that the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles are superparamagnetic with blocking temperatures below 78 K. The surfaces of the Sr{sub 3}Fe{sub 2}O{sub 6

  7. Depth Profiling Analysis of Aluminum Oxidation During Film Deposition in a Conventional High Vacuum System

    Science.gov (United States)

    Kim, Jongmin; Weimer, Jeffrey J.; Zukic, Muamer; Torr, Douglas G.

    1994-01-01

    The oxidation of aluminum thin films deposited in a conventional high vacuum chamber has been investigated using x-ray photoelectron spectroscopy (XPS) and depth profiling. The state of the Al layer was preserved by coating it with a protective MgF2 layer in the deposition chamber. Oxygen concentrations in the film layers were determined as a function of sputter time (depth into the film). The results show that an oxidized layer is formed at the start of Al deposition and that a less extensively oxidized Al layer is deposited if the deposition rate is fast. The top surface of the Al layer oxidizes very quickly. This top oxidized layer may be thicker than has been previously reported by optical methods. Maximum oxygen concentrations measured by XPS at each Al interface are related to pressure to rate ratios determined during the Al layer deposition.

  8. C:\\Users\\AISA\\Desktop\\XPS 26(1)\\OGNALAGA.xps

    African Journals Online (AJOL)

    AISA

    la dose apportée est élevée, plus la réaction positive des plants est grande. Les plants ... Moreover, the higher the supply dose, the greater the positive reaction of the .... Matériel organique. Les parties peu lignifiées des plantes C.odorata et L. leucocephalae, ont été récoltées et découpées à la machette afin de favoriser.

  9. Generation of a high-brightness pulsed positron beam for the Munich scanning positron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Piochacz, Christian

    2009-11-20

    Within the present work the prerequisites for the operation of the Munich scanning positron microscope (SPM) at the high intense neutron induced positron source Munich (NEPOMUC) were established. This was accomplished in two steps: Firstly, a re-moderation device was installed at the positron beam facility NEPOMUC, which enhances the brightness of the positron beam for all connected experiments. The second step was the design, set up and initial operation of the SPM interface for the high efficient conversion of the continuous beam into a bunched beam. The in-pile positron source NEPOMUC creates a positron beam with a diameter of typically 7 mm, a kinetic energy of 1 keV and an energy spread of 50 eV. The NEPOMUC re-moderator generates from this beam a low energy positron beam (20 - 200 eV) with a diameter of less than 2 mm and an energy spread well below 2.5 eV. This was achieved with an excellent total efficiency of 6.55{+-}0.25 %. The re-moderator was not only the rst step to implement the SPM at NEPOMUc, it enables also the operation of the pulsed low energy positron beam system (PLEPS). Within the present work, at this spectrometer rst positron lifetime measurements were performed, which revealed the defect types of an ion irradiated uranium molybdenum alloy. Moreover, the instruments which were already connected to the positron beam facility bene ts considerably of the high brightness enhancement. In the new SPM interface an additional re-moderation stage enhances the brightness of the beam even more and will enable positron lifetime measurements at the SPM with a lateral resolution below 1 {mu}m. The efficiency of the re-moderation process in this second stage was 24.5{+-}4.5 %. In order to convert high efficiently the continuous positron beam into a pulsed beam with a repetition rate of 50 MHz and a pulse duration of less than 50 ps, a sub-harmonic pre-bucher was combined with two sine wave bunchers. Furthermore, the additional re-moderation stage of the

  10. Generation of a high-brightness pulsed positron beam for the Munich scanning positron microscope

    International Nuclear Information System (INIS)

    Piochacz, Christian

    2009-01-01

    Within the present work the prerequisites for the operation of the Munich scanning positron microscope (SPM) at the high intense neutron induced positron source Munich (NEPOMUC) were established. This was accomplished in two steps: Firstly, a re-moderation device was installed at the positron beam facility NEPOMUC, which enhances the brightness of the positron beam for all connected experiments. The second step was the design, set up and initial operation of the SPM interface for the high efficient conversion of the continuous beam into a bunched beam. The in-pile positron source NEPOMUC creates a positron beam with a diameter of typically 7 mm, a kinetic energy of 1 keV and an energy spread of 50 eV. The NEPOMUC re-moderator generates from this beam a low energy positron beam (20 - 200 eV) with a diameter of less than 2 mm and an energy spread well below 2.5 eV. This was achieved with an excellent total efficiency of 6.55±0.25 %. The re-moderator was not only the rst step to implement the SPM at NEPOMUc, it enables also the operation of the pulsed low energy positron beam system (PLEPS). Within the present work, at this spectrometer rst positron lifetime measurements were performed, which revealed the defect types of an ion irradiated uranium molybdenum alloy. Moreover, the instruments which were already connected to the positron beam facility bene ts considerably of the high brightness enhancement. In the new SPM interface an additional re-moderation stage enhances the brightness of the beam even more and will enable positron lifetime measurements at the SPM with a lateral resolution below 1 μm. The efficiency of the re-moderation process in this second stage was 24.5±4.5 %. In order to convert high efficiently the continuous positron beam into a pulsed beam with a repetition rate of 50 MHz and a pulse duration of less than 50 ps, a sub-harmonic pre-bucher was combined with two sine wave bunchers. Furthermore, the additional re-moderation stage of the SPM

  11. Hydrothermal synthesis of highly nitrogen-doped few-layer graphene via solid–gas reaction

    International Nuclear Information System (INIS)

    Liang, Xianqing; Zhong, Jun; Shi, Yalin; Guo, Jin; Huang, Guolong; Hong, Caihao; Zhao, Yidong

    2015-01-01

    Highlights: • A novel approach to synthesis of N-doped few-layer graphene has been developed. • The high doping levels of N in products are achieved. • XPS and XANES results reveal a thermal transformation of N bonding configurations. • The developed method is cost-effective and eco-friendly. - Abstract: Nitrogen-doped (N-doped) graphene sheets with high doping concentration were facilely synthesized through solid–gas reaction of graphene oxide (GO) with ammonia vapor in a self-designed hydrothermal system. The morphology, surface chemistry and electronic structure of N-doped graphene sheets were investigated by TEM, AFM, XRD, XPS, XANES and Raman characterizations. Upon hydrothermal treatment, up to 13.22 at% of nitrogen could be introduced into the crumpled few-layer graphene sheets. Both XPS and XANES analysis reveal that the reaction between oxygen functional groups in GO and ammonia vapor produces amide and amine species in hydrothermally treated GO (HTGO). Subsequent thermal annealing of the resultant HTGO introduces a gradual transformation of nitrogen bonding configurations in graphene sheets from amine N to pyridinic and graphitic N with the increase of annealing temperature. This study provides a simple but cost-effective and eco-friendly method to prepare N-doped graphene materials in large-scale for potential applications

  12. High precision stress measurements in semiconductor structures by Raman microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Uhlig, Benjamin

    2009-07-01

    Stress in silicon structures plays an essential role in modern semiconductor technology. This stress has to be measured and due to the ongoing miniaturization in today's semiconductor industry, the measuring method has to meet certain requirements. The present thesis deals with the question how Raman spectroscopy can be used to measure the state of stress in semiconductor structures. In the first chapter the relation between Raman peakshift and stress in the material is explained. It is shown that detailed stress maps with a spatial resolution close to the diffraction limit can be obtained in structured semiconductor samples. Furthermore a novel procedure, the so called Stokes-AntiStokes-Difference method is introduced. With this method, topography, tool or drift effects can be distinguished from stress related influences in the sample. In the next chapter Tip-enhanced Raman Scattering (TERS) and its application for an improvement in lateral resolution is discussed. For this, a study is presented, which shows the influence of metal particles on the intensity and localization of the Raman signal. A method to attach metal particles to scannable tips is successfully applied. First TERS scans are shown and their impact on and challenges for high resolution stress measurements on semiconductor structures is explained. (orig.)

  13. Green Synthesis of Boron Carbonitride with High Capacitance

    Directory of Open Access Journals (Sweden)

    Dongping Chen

    2018-03-01

    Full Text Available Boron carbonitrides (BCN have attracted great interest in superhard or energy storage materials. In this work, thin BCN sheets were synthesized at 250 °C by a facile and green solvothermal method. The structure and morphology were characterized by X-ray diffraction (XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. Based on the results of electrochemical experiments, the thin BCN sheet exhibited excellent capacitance performance (343.1 F/g at a current density of 0.5 A/g and cycling stability (90%, which showed high potential applications in supercapacitors.

  14. High-resolution intravital microscopy.

    Directory of Open Access Journals (Sweden)

    Volker Andresen

    Full Text Available Cellular communication constitutes a fundamental mechanism of life, for instance by permitting transfer of information through synapses in the nervous system and by leading to activation of cells during the course of immune responses. Monitoring cell-cell interactions within living adult organisms is crucial in order to draw conclusions on their behavior with respect to the fate of cells, tissues and organs. Until now, there is no technology available that enables dynamic imaging deep within the tissue of living adult organisms at sub-cellular resolution, i.e. detection at the level of few protein molecules. Here we present a novel approach called multi-beam striped-illumination which applies for the first time the principle and advantages of structured-illumination, spatial modulation of the excitation pattern, to laser-scanning-microscopy. We use this approach in two-photon-microscopy--the most adequate optical deep-tissue imaging-technique. As compared to standard two-photon-microscopy, it achieves significant contrast enhancement and up to 3-fold improved axial resolution (optical sectioning while photobleaching, photodamage and acquisition speed are similar. Its imaging depth is comparable to multifocal two-photon-microscopy and only slightly less than in standard single-beam two-photon-microscopy. Precisely, our studies within mouse lymph nodes demonstrated 216% improved axial and 23% improved lateral resolutions at a depth of 80 µm below the surface. Thus, we are for the first time able to visualize the dynamic interactions between B cells and immune complex deposits on follicular dendritic cells within germinal centers (GCs of live mice. These interactions play a decisive role in the process of clonal selection, leading to affinity maturation of the humoral immune response. This novel high-resolution intravital microscopy method has a huge potential for numerous applications in neurosciences, immunology, cancer research and

  15. High-Resolution Intravital Microscopy

    Science.gov (United States)

    Andresen, Volker; Pollok, Karolin; Rinnenthal, Jan-Leo; Oehme, Laura; Günther, Robert; Spiecker, Heinrich; Radbruch, Helena; Gerhard, Jenny; Sporbert, Anje; Cseresnyes, Zoltan; Hauser, Anja E.; Niesner, Raluca

    2012-01-01

    Cellular communication constitutes a fundamental mechanism of life, for instance by permitting transfer of information through synapses in the nervous system and by leading to activation of cells during the course of immune responses. Monitoring cell-cell interactions within living adult organisms is crucial in order to draw conclusions on their behavior with respect to the fate of cells, tissues and organs. Until now, there is no technology available that enables dynamic imaging deep within the tissue of living adult organisms at sub-cellular resolution, i.e. detection at the level of few protein molecules. Here we present a novel approach called multi-beam striped-illumination which applies for the first time the principle and advantages of structured-illumination, spatial modulation of the excitation pattern, to laser-scanning-microscopy. We use this approach in two-photon-microscopy - the most adequate optical deep-tissue imaging-technique. As compared to standard two-photon-microscopy, it achieves significant contrast enhancement and up to 3-fold improved axial resolution (optical sectioning) while photobleaching, photodamage and acquisition speed are similar. Its imaging depth is comparable to multifocal two-photon-microscopy and only slightly less than in standard single-beam two-photon-microscopy. Precisely, our studies within mouse lymph nodes demonstrated 216% improved axial and 23% improved lateral resolutions at a depth of 80 µm below the surface. Thus, we are for the first time able to visualize the dynamic interactions between B cells and immune complex deposits on follicular dendritic cells within germinal centers (GCs) of live mice. These interactions play a decisive role in the process of clonal selection, leading to affinity maturation of the humoral immune response. This novel high-resolution intravital microscopy method has a huge potential for numerous applications in neurosciences, immunology, cancer research and developmental biology

  16. Ex-situ XPS-investigation of the interface between PE-CVD SiO{sub 2} and wet chemically etched MO-CVD epitaxial layers of In{sub 0.53}Ga{sub 0.47}As

    Energy Technology Data Exchange (ETDEWEB)

    Procop, M. [Bundesanstalt fuer Materialforschung und -pruefung, Berlin (Germany); Wandel, K. [Humboldt-Universitaet, Berlin (Germany). Inst. fuer Festkoerperphysik; Verucchi, R. [Modena Univ. (Italy). Ist. di Fisica

    1995-11-01

    The As rich SiO{sub 2}/In{sub 0.53}Ga{sub 0.47}As interface which is produced by wet chemical etching before SiO{sub 2} deposition to improve the electronic properties of the interface has been studied. SiO{sub 2}-layers of about 10 to 20 nm thickness have been deposited in a plasma enhanced chemical vapour deposition (PECVD) reactor and then thinned down to about 4 to 3 nm by 1.5 keV Ar ion beam bombardment at grazing incidence (85 ) in the XPS analysis chamber. The photoelectron spectra show that an additional broadening of the In and As lines due to a possible ion beam damage can be neglected in case of a qualitative interpretation of the interface spectra. Moreover, TRIM simulations of the collision cascade reveal low damage production in the SiO{sub 2}/In{sub 0.53}Ga{sub 0.47}As interface region. Therefore such ex-situ XPS experiments allow a supervision of the interface chemistry after the fabrication process and an optimisation of the technology with regard to the etching solution and deposition conditions. The conservation or removal of the elemental arsenic and the oxidation of the semiconductor due to the SiO{sub 2} deposition are well reflected in the photoelectron spectra. (orig.)

  17. Composition Dependence of the Na(+) Ion Conductivity in 0.5Na2S + 0.5[xGeS2 + (1 - x)PS5/2] Mixed Glass Former Glasses: A Structural Interpretation of a Negative Mixed Glass Former Effect.

    Science.gov (United States)

    Martin, Steve W; Bischoff, Christian; Schuller, Katherine

    2015-12-24

    A negative mixed glass former effect (MGFE) in the Na(+) ion conductivity of glass has been found in 0.5Na2S + 0.5[xGeS2 + (1 - x)PS5/2] glasses where the Na(+) ion conductivity is significantly smaller for all of the ternary glasses than either of the binary end-member glasses. The minimum conductivity of ∼0.4 × 10(-6) (Ω cm)(-1) at 25 °C occurs for the x = 0.7 glass. Prior to this observation, the alkali ion conductivity of sulfide glasses at constant alkali concentration, but variable ratio of one glass former for another (x) ternary mixed glass former (MGF) glasses, has always produced a positive MGFE in the alkali ion conductivity; that is, the ternary glasses have always had higher ion conductivities that either of the end-member binary glasses. While the Na(+) ion conductivity exhibits a single global minimum value, the conductivity activation energy exhibits a bimodal double maximum at x ≈ 0.4 and x ≈ 0.7. The modified Christensen-Martin-Anderson-Stuart (CMAS) model of the activation energies reveals the origin of the negative MGFE to be due to an increase in the dielectric stiffness (a decrease in relative dielectric permittivity) of these glasses. When coupled with an increase in the average Na(+) ion jump distance and a slight increase in the mechanical stiffness of the glass, this causes the activation energy to go through maximum values and thereby produce the negative MGFE. The double maximum in the conductivity activation energy is coincident with double maximums in CMAS calculated strain, ΔES, and Coulombic, ΔEC, activation energies. In these ternary glasses, the increase in the dielectric stiffness of the glass arises from a negative deviation of the limiting high frequency dielectric permittivity as compared to the binary end-member glasses. While the CMAS calculated total activation energies ΔEact = ΔES + ΔEC are found to reproduce the overall shape of the composition dependence of the measured ΔEact values, they are consistently

  18. A combined ToF-SIMS and XPS study for the elucidation of the role of water in the performances of a Post-Plasma Process using LaMnO3+δ as catalyst in the total oxidation of trichloroethylene

    Science.gov (United States)

    Nuns, N.; Beaurain, A.; Dinh, M. T. Nguyen; Vandenbroucke, A.; De Geyter, N.; Morent, R.; Leys, C.; Giraudon, J.-M.; Lamonier, J.-F.

    2014-11-01

    LaMnO3+δ which is an environment-friendly and inexpensive material has been previously used as catalyst in Post-Plasma Catalysis (PPC) in the total oxidation of trichloroethylene (TCE) which is a solvent widely used in dry cleaning and degreasing processes. It has been shown that the process efficiency increases in moist air (RH = 18%).The issue we want to address herein is the effect of water on the location of chlorine at the surface of the catalyst as chlorine is able to alter the catalyst structure, activity and stability. Therefore, a combined Time of Flight-Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) study has been carried out on the fresh LaMnO3+δ catalyst (LM) and used catalysts after performing PPC with TCE diluted in dry synthetic air (LM0) or with industrial air containing water (LM18; 18 stands for the Relative Humidity) and CO2 (about 560 ppmv) at a temperature of 150 °C. XPS and ToF-SIMS results both show the presence of chlorine on the tested catalysts whose amount increases by exposure of the catalyst to the reactive mixture in dry synthetic air. XPS results reveal that chlorine is present as both chloride ion and covalent chlorine on LM0 while organic chlorinated residues are absent on LM18 catalyst. ToF-SIMS study indicates that lanthanum excess as oxide(hydroxide) partially covering the perovskite mainly transforms into LaOCl and to a minor extent into LaCl3. Extent of Mn chlorination seems to be favored over LM0 having a higher MnClx±/MnOCl± ionic ratio compared to LM18. Furthermore ToF-SIMS clearly identifies C1 chlorinated organic ions, mainly CH2Cl+ and CHCl2-, on LM0 which may contribute to the XPS Cl organic component. From the combined ToF-SIMS and XPS results it is found that water delays the surface degradation extent of the perovskite into related (oxy)(hydroxy)chlorinated inorganic phases by less molecular chlorine and related chlorine species on the catalyst surface. A reaction scheme of

  19. A combined ToF-SIMS and XPS study for the elucidation of the role of water in the performances of a Post-Plasma Process using LaMnO3+δ as catalyst in the total oxidation of trichloroethylene

    International Nuclear Information System (INIS)

    Nuns, N.; Beaurain, A.; Dinh, M.T. Nguyen; Vandenbroucke, A.; De Geyter, N.; Morent, R.; Leys, C.; Giraudon, J.-M.; Lamonier, J.-F.

    2014-01-01

    Graphical abstract: - Highlights: • Water promotes the cleaning of the perovskite active sites. • Water is able to tune the degradation pathway of dichloroacetyl chloride. • Detection of CH 2 Cl + and CHCl 2 + by ToF-SIMS on the catalyst in dry air. - Abstract: LaMnO 3+δ which is an environment-friendly and inexpensive material has been previously used as catalyst in Post-Plasma Catalysis (PPC) in the total oxidation of trichloroethylene (TCE) which is a solvent widely used in dry cleaning and degreasing processes. It has been shown that the process efficiency increases in moist air (RH = 18%).The issue we want to address herein is the effect of water on the location of chlorine at the surface of the catalyst as chlorine is able to alter the catalyst structure, activity and stability. Therefore, a combined Time of Flight-Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) study has been carried out on the fresh LaMnO 3+δ catalyst (LM) and used catalysts after performing PPC with TCE diluted in dry synthetic air (LM0) or with industrial air containing water (LM18; 18 stands for the Relative Humidity) and CO 2 (about 560 ppmv) at a temperature of 150 °C. XPS and ToF-SIMS results both show the presence of chlorine on the tested catalysts whose amount increases by exposure of the catalyst to the reactive mixture in dry synthetic air. XPS results reveal that chlorine is present as both chloride ion and covalent chlorine on LM0 while organic chlorinated residues are absent on LM18 catalyst. ToF-SIMS study indicates that lanthanum excess as oxide(hydroxide) partially covering the perovskite mainly transforms into LaOCl and to a minor extent into LaCl 3 . Extent of Mn chlorination seems to be favored over LM0 having a higher MnCl x ± /MnOCl ± ionic ratio compared to LM18. Furthermore ToF-SIMS clearly identifies C1 chlorinated organic ions, mainly CH 2 Cl + and CHCl 2 − , on LM0 which may contribute to the XPS Cl organic

  20. A combined ToF-SIMS and XPS study for the elucidation of the role of water in the performances of a Post-Plasma Process using LaMnO{sub 3+δ} as catalyst in the total oxidation of trichloroethylene

    Energy Technology Data Exchange (ETDEWEB)

    Nuns, N. [Université Lille1 Sciences et Technologies, Lille (France); IMMCL Chevreul, Institut des Molécules et de la Matière Condensée, Lille (France); Beaurain, A. [Université Lille1 Sciences et Technologies, Lille (France); Dinh, M.T. Nguyen [Université Lille1 Sciences et Technologies, Lille (France); Unité de Catalyse et de Chimie du Solide, UMR CNRS 8181, 59655 Villeneuve d’Ascq (France); Vandenbroucke, A.; De Geyter, N.; Morent, R.; Leys, C. [Research Unit Plasma Technology, Departement of Applied Physics, Ghent University (Belgium); Giraudon, J.-M., E-mail: jean-marc.giraudon@univ-lille1.fr [Université Lille1 Sciences et Technologies, Lille (France); Unité de Catalyse et de Chimie du Solide, UMR CNRS 8181, 59655 Villeneuve d’Ascq (France); Lamonier, J.-F. [Université Lille1 Sciences et Technologies, Lille (France); Unité de Catalyse et de Chimie du Solide, UMR CNRS 8181, 59655 Villeneuve d’Ascq (France)

    2014-11-30

    Graphical abstract: - Highlights: • Water promotes the cleaning of the perovskite active sites. • Water is able to tune the degradation pathway of dichloroacetyl chloride. • Detection of CH{sub 2}Cl{sup +} and CHCl{sub 2}{sup +} by ToF-SIMS on the catalyst in dry air. - Abstract: LaMnO{sub 3+δ} which is an environment-friendly and inexpensive material has been previously used as catalyst in Post-Plasma Catalysis (PPC) in the total oxidation of trichloroethylene (TCE) which is a solvent widely used in dry cleaning and degreasing processes. It has been shown that the process efficiency increases in moist air (RH = 18%).The issue we want to address herein is the effect of water on the location of chlorine at the surface of the catalyst as chlorine is able to alter the catalyst structure, activity and stability. Therefore, a combined Time of Flight-Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) study has been carried out on the fresh LaMnO{sub 3+δ} catalyst (LM) and used catalysts after performing PPC with TCE diluted in dry synthetic air (LM0) or with industrial air containing water (LM18; 18 stands for the Relative Humidity) and CO{sub 2} (about 560 ppmv) at a temperature of 150 °C. XPS and ToF-SIMS results both show the presence of chlorine on the tested catalysts whose amount increases by exposure of the catalyst to the reactive mixture in dry synthetic air. XPS results reveal that chlorine is present as both chloride ion and covalent chlorine on LM0 while organic chlorinated residues are absent on LM18 catalyst. ToF-SIMS study indicates that lanthanum excess as oxide(hydroxide) partially covering the perovskite mainly transforms into LaOCl and to a minor extent into LaCl{sub 3}. Extent of Mn chlorination seems to be favored over LM0 having a higher MnCl{sub x}{sup ±}/MnOCl{sup ±} ionic ratio compared to LM18. Furthermore ToF-SIMS clearly identifies C1 chlorinated organic ions, mainly CH{sub 2}Cl{sup +} and CHCl

  1. Novel protocol for highly efficient gas-phase chemical derivatization of surface amine groups using trifluoroacetic anhydride

    Science.gov (United States)

    Duchoslav, Jiri; Kehrer, Matthias; Hinterreiter, Andreas; Duchoslav, Vojtech; Unterweger, Christoph; Fürst, Christian; Steinberger, Roland; Stifter, David

    2018-06-01

    In the current work, chemical derivatization of amine (NH2) groups with trifluoroacetic anhydride (TFAA) as an analytical method to improve the information scope of X-ray photoelectron spectroscopy (XPS) is investigated. TFAA is known to successfully label hydroxyl (OH) groups. With the introduction of a newly developed gas-phase derivatization protocol conducted at ambient pressure and using a catalyst also NH2 groups can now efficiently be labelled with a high yield and without the formation of unwanted by-products. By establishing a comprehensive and self-consistent database of reference binding energies for XPS a promising approach for distinguishing hydroxyl from amine groups is presented. The protocol was verified on different polymers, including poly(allylamine), poly(ethyleneimine), poly(vinylalcohol) and chitosan, the latter one containing both types of addressed chemical groups.

  2. Structure, Mobility, and Composition of Transition Metal Catalyst Surfaces. High-Pressure Scanning Tunneling Microscopy and Ambient-Pressure X-ray Photoelectron Spectroscopy Studies

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Zhongwei [Univ. of California, Berkeley, CA (United States)

    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.

  3. Epitaxial deposition of silver ultrafine nano-clusters on defect-free surfaces of HOPG-derived few-layer graphene in a UHV multi-chamber by in-situ STM, ex-situ XPS and ab initio calculations

    CSIR Research Space (South Africa)

    Ndlovu, GF

    2012-03-01

    Full Text Available The growth of three-dimensional ultra-fine spherical nano-particles of silver on few layers of graphene derived from highly oriented pyrolytic graphite in ultra-high vacuum were characterized using in situ scanning tunneling microscopy (STM...

  4. High-throughput characterization for solar fuels materials discovery

    Science.gov (United States)

    Mitrovic, Slobodan; Becerra, Natalie; Cornell, Earl; Guevarra, Dan; Haber, Joel; Jin, Jian; Jones, Ryan; Kan, Kevin; Marcin, Martin; Newhouse, Paul; Soedarmadji, Edwin; Suram, Santosh; Xiang, Chengxiang; Gregoire, John; High-Throughput Experimentation Team

    2014-03-01

    In this talk I will present the status of the High-Throughput Experimentation (HTE) project of the Joint Center for Artificial Photosynthesis (JCAP). JCAP is an Energy Innovation Hub of the U.S. Department of Energy with a mandate to deliver a solar fuel generator based on an integrated photoelectrochemical cell (PEC). However, efficient and commercially viable catalysts or light absorbers for the PEC do not exist. The mission of HTE is to provide the accelerated discovery through combinatorial synthesis and rapid screening of material properties. The HTE pipeline also features high-throughput material characterization using x-ray diffraction and x-ray photoemission spectroscopy (XPS). In this talk I present the currently operating pipeline and focus on our combinatorial XPS efforts to build the largest free database of spectra from mixed-metal oxides, nitrides, sulfides and alloys. This work was performed at Joint Center for Artificial Photosynthesis, a DOE Energy Innovation Hub, supported through the Office of Science of the U.S. Department of Energy under Award No. DE-SC0004993.

  5. Growth and characterization of stoichiometric BCN films on highly oriented pyrolytic graphite by radiofrequency plasma enhanced chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Mannan, Md. Abdul, E-mail: amannan75@yahoo.co [Department of Chemistry and Applied Chemistry, Faculty of Science and Engineering, Saga University, 1 Honjo, Saga 840-8502 (Japan); Synchrotron Radiation Research Unit, Quantum Beam Science Directorate, Japan Atomic Energy Agency, Tokai-mura, Naka-gun, Ibaraki 319-1195 (Japan); Noguchi, Hideyuki; Kida, Tetsuya; Nagano, Masamitsu [Department of Chemistry and Applied Chemistry, Faculty of Science and Engineering, Saga University, 1 Honjo, Saga 840-8502 (Japan); Hirao, Norie; Baba, Yuji [Synchrotron Radiation Research Unit, Quantum Beam Science Directorate, Japan Atomic Energy Agency, Tokai-mura, Naka-gun, Ibaraki 319-1195 (Japan)

    2010-05-31

    Hexagonal boron carbonitride (h-BCN) hybrid films have been synthesized on highly oriented pyrolytic graphite by radiofrequency plasma enhanced chemical vapor deposition using tris-(dimethylamino)borane as a single-source molecular precursor. The films were characterized by X-ray photoelectron spectroscopy (XPS), near-edge X-ray absorption fine structure (NEXAFS) and Raman spectroscopic measurements. XPS measurement showed that the B atoms were bonded to C and N atoms to form the sp{sup 2}-B-C-N atomic hybrid chemical environment. The atomic composition estimated from the XPS of the typical sample was found to be almost B{sub 1}C{sub 1}N{sub 1}. NEXAFS spectra of the B K-edge and the N K-edge had the peaks due to the {pi}* and {sigma}* resonances of sp{sup 2} hybrid orbitals implying the existence of the sp{sup 2} hybrid configurations of h-BCN around the B atoms. The G band at 1592 and D band at 1352 cm{sup -1} in the Raman spectra also suggested the presence of the graphite-like sp{sup 2}-B-C-N atomic hybrid bonds. The films consisted of micrometer scale crystalline structure of around 10 {mu}m thick has been confirmed by the field emission scanning electron microscopy.

  6. Progress in the fabrication of high aspect ratio zone plates by soft x-ray lithography

    International Nuclear Information System (INIS)

    Divan, R.; Mancini, D. C.; Moldovan, N. A.; Lai, B.; Assoufid, L.; Leondard, Q.; Cerrina, F.

    2002-01-01

    Fabrication of Fresnel zone plates for the hard x-ray spectral region combines the challenge of high lateral resolution (∼100 nm) with a large thickness requirement for the phase-shifting material (0.5-3 (micro)m). For achieving a high resolution, the initial mask was fabricated by e-beam lithography and gold electroforming. To prevent the collapse of the structures between the developing and electroforming processes, drying was completely eliminated. Fabrication errors, such as nonuniform gold electroplating and collapse of structures, were systematically analyzed and largely eliminated. We optimized the exposure and developing processes for 950k and 2200k polymethylmethacrylate of different thicknesses and various adhesion promoters. We discuss the effects of these fabrication steps on the zone plate's resolution and aspect ratio. Fresnel zone plates with 110 nm outermost zone width, 150 (micro)m diameter, and 1.3 (micro)m gold thickness were fabricated. Preliminary evaluation of the FZPs was done by scanning electron microscopy and atomic force microscopy. The FZP focusing performance was characterized at the Advanced Photon Source at Argonne National Laboratory

  7. Characterizing the optical properties of human brain tissue with high numerical aperture optical coherence tomography.

    Science.gov (United States)

    Wang, Hui; Magnain, Caroline; Sakadžić, Sava; Fischl, Bruce; Boas, David A

    2017-12-01

    Quantification of tissue optical properties with optical coherence tomography (OCT) has proven to be useful in evaluating structural characteristics and pathological changes. Previous studies primarily used an exponential model to analyze low numerical aperture (NA) OCT measurements and obtain the total attenuation coefficient for biological tissue. In this study, we develop a systematic method that includes the confocal parameter for modeling the depth profiles of high NA OCT, when the confocal parameter cannot be ignored. This approach enables us to quantify tissue optical properties with higher lateral resolution. The model parameter predictions for the scattering coefficients were tested with calibrated microsphere phantoms. The application of the model to human brain tissue demonstrates that the scattering and back-scattering coefficients each provide unique information, allowing us to differentially identify laminar structures in primary visual cortex and distinguish various nuclei in the midbrain. The combination of the two optical properties greatly enhances the power of OCT to distinguish intricate structures in the human brain beyond what is achievable with measured OCT intensity information alone, and therefore has the potential to enable objective evaluation of normal brain structure as well as pathological conditions in brain diseases. These results represent a promising step for enabling the quantification of tissue optical properties from high NA OCT.

  8. Visualization of the microcirculatory network in skin by high frequency optoacoustic mesoscopy

    Science.gov (United States)

    Schwarz, Mathias; Aguirre, Juan; Buehler, Andreas; Omar, Murad; Ntziachristos, Vasilis

    2015-07-01

    Optoacoustic (photoacoustic) imaging has a high potential for imaging melanin-rich structures in skin and the microvasculature of the dermis due to the natural chromophores (de)oxyhemoglobin, and melanin. The vascular network in human dermis comprises a large network of arterioles, capillaries, and venules, ranging from 5 μm to more than 100 μm in diameter. The frequency spectrum of the microcirculatory network in human skin is intrinsically broadband, due to the large variety in size of absorbers. In our group we have developed raster-scan optoacoustic mesoscopy (RSOM) that applies a 100 MHz transducer with ultra-wide bandwidth in raster-scan mode achieving lateral resolution of 18 μm. In this study, we applied high frequency RSOM to imaging human skin in a healthy volunteer. We analyzed the frequency spectrum of anatomical structures with respect to depth and show that frequencies >60 MHz contain valuable information of structures in the epidermis and the microvasculature of the papillary dermis. We illustrate that RSOM is capable of visualizing the fine vascular network at and beneath the epidermal-dermal junction, revealing the vascular fingerprint of glabrous skin, as well as the larger venules deeper inside the dermis. We evaluate the ability of the RSOM system in measuring epidermal thickness in both hairy and glabrous skin. Finally, we showcase the capability of RSOM in visualizing benign nevi that will potentially help in imaging the penetration depth of melanoma.

  9. Stand-alone front-end system for high- frequency, high-frame-rate coded excitation ultrasonic imaging.

    Science.gov (United States)

    Park, Jinhyoung; Hu, Changhong; Shung, K Kirk

    2011-12-01

    A stand-alone front-end system for high-frequency coded excitation imaging was implemented to achieve a wider dynamic range. The system included an arbitrary waveform amplifier, an arbitrary waveform generator, an analog receiver, a motor position interpreter, a motor controller and power supplies. The digitized arbitrary waveforms at a sampling rate of 150 MHz could be programmed and converted to an analog signal. The pulse was subsequently amplified to excite an ultrasound transducer, and the maximum output voltage level achieved was 120 V(pp). The bandwidth of the arbitrary waveform amplifier was from 1 to 70 MHz. The noise figure of the preamplifier was less than 7.7 dB and the bandwidth was 95 MHz. Phantoms and biological tissues were imaged at a frame rate as high as 68 frames per second (fps) to evaluate the performance of the system. During the measurement, 40-MHz lithium niobate (LiNbO(3)) single-element lightweight (<;0.28 g) transducers were utilized. The wire target measure- ment showed that the -6-dB axial resolution of a chirp-coded excitation was 50 μm and lateral resolution was 120 μm. The echo signal-to-noise ratios were found to be 54 and 65 dB for the short burst and coded excitation, respectively. The contrast resolution in a sphere phantom study was estimated to be 24 dB for the chirp-coded excitation and 15 dB for the short burst modes. In an in vivo study, zebrafish and mouse hearts were imaged. Boundaries of the zebrafish heart in the image could be differentiated because of the low-noise operation of the implemented system. In mouse heart images, valves and chambers could be readily visualized with the coded excitation.

  10. High temperature reactions between molybdenum and metal halides

    International Nuclear Information System (INIS)

    Boeroeczki, A.; Dobos, G.; Josepovits, V.K.; Hars, Gy.

    2006-01-01

    Good colour rendering properties, high intensity and efficacy are of vital importance for high-end lighting applications. These requirements can be achieved by high intensity discharge lamps doped with different metal halide additives (metal halide lamps). To improve their reliability, it is very important to understand the different failure processes of the lamps. In this paper, the corrosion reactions between different metal halides and the molybdenum electrical feed-through electrode are discussed. The reactions were studied in the feed-through of real lamps and on model samples too. X-ray photoelectron spectroscopy (XPS) was used to establish the chemical states. In case of the model samples we have also used atomic absorption spectroscopy (AAS) to measure the reaction product amounts. Based on the measurement results we were able to determine the most corrosive metal halide components and to understand the mechanism of the reactions

  11. High-resolution non-destructive three-dimensional imaging of integrated circuits

    Science.gov (United States)

    Holler, Mirko; Guizar-Sicairos, Manuel; Tsai, Esther H. R.; Dinapoli, Roberto; Müller, Elisabeth; Bunk, Oliver; Raabe, Jörg; Aeppli, Gabriel

    2017-03-01

    Modern nanoelectronics has advanced to a point at which it is impossible to image entire devices and their interconnections non-destructively because of their small feature sizes and the complex three-dimensional structures resulting from their integration on a chip. This metrology gap implies a lack of direct feedback between design and manufacturing processes, and hampers quality control during production, shipment and use. Here we demonstrate that X-ray ptychography—a high-resolution coherent diffractive imaging technique—can create three-dimensional images of integrated circuits of known and unknown designs with a lateral resolution in all directions down to 14.6 nanometres. We obtained detailed device geometries and corresponding elemental maps, and show how the devices are integrated with each other to form the chip. Our experiments represent a major advance in chip inspection and reverse engineering over the traditional destructive electron microscopy and ion milling techniques. Foreseeable developments in X-ray sources, optics and detectors, as well as adoption of an instrument geometry optimized for planar rather than cylindrical samples, could lead to a thousand-fold increase in efficiency, with concomitant reductions in scan times and voxel sizes.

  12. High-resolution non-destructive three-dimensional imaging of integrated circuits.

    Science.gov (United States)

    Holler, Mirko; Guizar-Sicairos, Manuel; Tsai, Esther H R; Dinapoli, Roberto; Müller, Elisabeth; Bunk, Oliver; Raabe, Jörg; Aeppli, Gabriel

    2017-03-15

    Modern nanoelectronics has advanced to a point at which it is impossible to image entire devices and their interconnections non-destructively because of their small feature sizes and the complex three-dimensional structures resulting from their integration on a chip. This metrology gap implies a lack of direct feedback between design and manufacturing processes, and hampers quality control during production, shipment and use. Here we demonstrate that X-ray ptychography-a high-resolution coherent diffractive imaging technique-can create three-dimensional images of integrated circuits of known and unknown designs with a lateral resolution in all directions down to 14.6 nanometres. We obtained detailed device geometries and corresponding elemental maps, and show how the devices are integrated with each other to form the chip. Our experiments represent a major advance in chip inspection and reverse engineering over the traditional destructive electron microscopy and ion milling techniques. Foreseeable developments in X-ray sources, optics and detectors, as well as adoption of an instrument geometry optimized for planar rather than cylindrical samples, could lead to a thousand-fold increase in efficiency, with concomitant reductions in scan times and voxel sizes.

  13. Potassium and soot interaction in fast biomass pyrolysis at high temperatures

    DEFF Research Database (Denmark)

    Trubetskaya, Anna; Hofmann Larsen, Flemming; Shchukarev, Andrey

    2018-01-01

    2 reactivity was studied by thermogravimetric analysis. The XPS results showed that potassium incorporation with oxygen-containing surface groups in the soot matrix did not occur during high temperature pyrolysis. The potassium was mostly found as water-soluble salts such as KCl, KOH, KHCO3 and K2CO...... potassium amount was incorporated in the soot matrix during pyrolysis. Raman spectroscopy results showed that the carbon chemistry of biomass soot also affected the CO2 reactivity. The less reactive pinewood soot was more graphitic than herbaceous biomass soot samples with the disordered carbon structure...

  14. Activated carbon derived from harmful aquatic plant for high stable supercapacitors

    Science.gov (United States)

    Li, Jiangfeng; Wu, Qingsheng

    2018-01-01

    Considering cost and environmental protection, the harmful aquatic plant altemanthera philoxeroides derived carbon material with super high specific surface area (2895 m2 g-1) is an ideal electrode material for supercapacitor. The structure and composition of these carbon materials were characterized by SEM, EDS, XPS and BET measurements. The obtained material exhibits a maximum specific capacitance of 275 F g-1 at 0.5 A g-1 and retains a capacitance of 210 F g-1 even at 50 A g-1. In addition, it also shows excellent capacity retention of 5000 cycles at 10 A g-1.

  15. Hydrothermal Synthesis and Biocompatibility Study of Highly Crystalline Carbonated Hydroxyapatite Nanorods

    Science.gov (United States)

    Xue, Caibao; Chen, Yingzhi; Huang, Yongzhuo; Zhu, Peizhi

    2015-08-01

    Highly crystalline carbonated hydroxyapatite (CHA) nanorods with different carbonate contents were synthesized by a novel hydrothermal method. The crystallinity and chemical structure of synthesized nanorods were studied by Fourier transform infrared spectroscopy (FTIR), X-ray photo-electronic spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM). The biocompatibility of synthesized CHA nanorods was evaluated by cell viability and alkaline phosphatase (ALP) activity of MG-63 cell line. The biocompatibility evaluation results show that these CHA nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopedic application.

  16. Effect of High-Temperature Annealing on Yellow and Blue Luminescence of Undoped GaN

    International Nuclear Information System (INIS)

    Chai Xu-Zhao; Zhou Dong; Liu Bin; Xie Zi-Li; Han Ping; Xiu Xiang-Qian; Chen Peng; Lu Hai; Zhang Rong; Zheng You-Dou

    2015-01-01

    The effect of high-temperature annealing on the yellow and blue luminescence of the undoped GaN is investigated by photoluminescence (PL) and x-ray photoelectron spectroscopy (XPS). It is found that the band-edge emission in the GaN apparently increases, and the yellow luminescence (YL) and blue luminescence (BL) bands dramatically decrease after annealing at 700°C. At the annealing temperature higher than 900°C, the YL and BL intensities show an enhancement for the nitrogen annealed GaN. This fact should be attributed to the increment of the Ga and N vacancies in the GaN decomposition. However, the integrated PL intensity of the oxygen annealed GaN decreases at the temperature ranging from 900°C to 1000°C. This results from the capture of many photo-generated holes by high-density surface states. XPS characterization confirms that the high-density surface states mainly originate from the incorporation of oxygen atoms into GaN at the high annealing temperature, and even induces the 0.34eV increment of the upward band bending for the oxygen annealed GaN at 1000°C. (paper)

  17. Amide group anchored glucose oxidase based anodic catalysts for high performance enzymatic biofuel cell

    Science.gov (United States)

    Chung, Yongjin; Ahn, Yeonjoo; Kim, Do-Heyoung; Kwon, Yongchai

    2017-01-01

    A new enzyme catalyst is formed by fabricating gold nano particle (GNP)-glucose oxidase (GOx) clusters that are then attached to polyethyleneimine (PEI) and carbon nanotube (CNT) with cross-linkable terephthalaldehyde (TPA) (TPA/[CNT/PEI/GOx-GNP]). Especially, amide bonds belonging to TPA play an anchor role for incorporating rigid bonding among GNP, GOx and CNT/PEI, while middle size GNP is well bonded with thiol group of GOx to form strong GNP-GOx cluster. Those bonds are identified by chemical and electrochemical characterizations like XPS and cyclic voltammogram. The anchording effect of amide bonds induces fast electron transfer and strong chemical bonding, resulting in enhancements in (i) catalytic activity, (ii) amount of immobilized GOx and (ii) performance of enzymatic biofuel cell (EBC) including the catalyst. Regarding the catalytic activity, the TPA/[CNT/PEI/GOx-GNP] produces high electron transfer rate constant (6 s-1), high glucose sensitivity (68 μA mM-1 cm-2), high maximum current density (113 μA cm-2), low charge transfer resistance (17.0 Ω cm2) and long-lasting durability while its chemical structure is characterized by XPS confirming large portion of amide bond. In EBC measurement, it has high maximum power density (0.94 mW cm-2) compatible with catalytic acitivity measurements.

  18. The influence of methanol on the chemical state of PtRu anodes in a high-temperature direct methanol fuel cell studied in situ by synchrotron-based near-ambient pressure x-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Saveleva, Viktoriia A; Savinova, Elena R; Daletou, Maria K

    2017-01-01

    Synchrotron radiation-based near-ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) has recently become a powerful tool for the investigation of interfacial phenomena in electrochemical power sources such as batteries and fuel cells. Here we present an in situ NAP-XPS study of the anode of a high-temperature direct methanol fuel cell with a phosphoric acid-doped hydrocarbon membrane, which reveals an enhanced flooding of the Pt 3 Ru anode with phosphoric acid in the presence of methanol. An analysis of the electrode surface composition depending on the cell voltage and on the presence of methanol reveals the strong influence of the latter on the extent of Pt oxidation and on the transformation of Ru into Ru (IV) hydroxide. (paper)

  19. The influence of methanol on the chemical state of PtRu anodes in a high-temperature direct methanol fuel cell studied in situ by synchrotron-based near-ambient pressure x-ray photoelectron spectroscopy

    Science.gov (United States)

    Saveleva, Viktoriia A.; Daletou, Maria K.; Savinova, Elena R.

    2017-01-01

    Synchrotron radiation-based near-ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) has recently become a powerful tool for the investigation of interfacial phenomena in electrochemical power sources such as batteries and fuel cells. Here we present an in situ NAP-XPS study of the anode of a high-temperature direct methanol fuel cell with a phosphoric acid-doped hydrocarbon membrane, which reveals an enhanced flooding of the Pt3Ru anode with phosphoric acid in the presence of methanol. An analysis of the electrode surface composition depending on the cell voltage and on the presence of methanol reveals the strong influence of the latter on the extent of Pt oxidation and on the transformation of Ru into Ru (IV) hydroxide.

  20. Highly active engineered-enzyme oriented monolayers: formation, characterization and sensing applications

    Directory of Open Access Journals (Sweden)

    Patolsky Fernando

    2011-06-01

    Full Text Available Abstract Background The interest in introducing ecologically-clean, and efficient enzymes into modern industry has been growing steadily. However, difficulties associated with controlling their orientation, and maintaining their selectivity and reactivity is still a significant obstacle. We have developed precise immobilization of biomolecules, while retaining their native functionality, and report a new, fast, easy, and reliable procedure of protein immobilization, with the use of Adenylate kinase as a model system. Methods Self-assembled monolayers of hexane-1,6-dithiol were formed on gold surfaces. The monolayers were characterized by contact-angle measurements, Elman-reagent reaction, QCM, and XPS. A specifically designed, mutated Adenylate kinase, where cysteine was inserted at the 75 residue, and the cysteine at residue 77 was replaced by serine, was used for attachment to the SAM surface via spontaneously formed disulfide (S-S bonds. QCM, and XPS were used for characterization of the immobilized protein layer. Curve fitting in XPS measurements used a Gaussian-Lorentzian function. Results and Discussion Water contact angle (65-70°, as well as all characterization techniques used, confirmed the formation of self-assembled monolayer with surface SH groups. X-ray photoelectron spectroscopy showed clearly the two types of sulfur atom, one attached to the gold (triolate and the other (SH/S-S at the ω-position for the hexane-1,6-dithiol SAMs. The formation of a protein monolayer was confirmed using XPS, and QCM, where the QCM-determined amount of protein on the surface was in agreement with a model that considered the surface area of a single protein molecule. Enzymatic activity tests of the immobilized protein confirmed that there is no change in enzymatic functionality, and reveal activity ~100 times that expected for the same amount of protein in solution. Conclusions To the best of our knowledge, immobilization of a protein by the method

  1. Investigation of significantly high barrier height in Cu/GaN Schottky diode

    Directory of Open Access Journals (Sweden)

    Manjari Garg

    2016-01-01

    Full Text Available Current-voltage (I-V measurements combined with analytical calculations have been used to explain mechanisms for forward-bias current flow in Copper (Cu Schottky diodes fabricated on Gallium Nitride (GaN epitaxial films. An ideality factor of 1.7 was found at room temperature (RT, which indicated deviation from thermionic emission (TE mechanism for current flow in the Schottky diode. Instead the current transport was better explained using the thermionic field-emission (TFE mechanism. A high barrier height of 1.19 eV was obtained at room temperature. X-ray photoelectron spectroscopy (XPS was used to investigate the plausible reason for observing Schottky barrier height (SBH that is significantly higher than as predicted by the Schottky-Mott model for Cu/GaN diodes. XPS measurements revealed the presence of an ultrathin cuprous oxide (Cu2O layer at the interface between Cu and GaN. With Cu2O acting as a degenerate p-type semiconductor with high work function of 5.36 eV, a high barrier height of 1.19 eV is obtained for the Cu/Cu2O/GaN Schottky diode. Moreover, the ideality factor and barrier height were found to be temperature dependent, implying spatial inhomogeneity of barrier height at the metal semiconductor interface.

  2. High-resolution noncontact AFM and Kelvin probe force microscopy investigations of self-assembled photovoltaic donor–acceptor dyads

    Directory of Open Access Journals (Sweden)

    Benjamin Grévin

    2016-06-01

    Full Text Available Self-assembled donor–acceptor dyads are used as model nanostructured heterojunctions for local investigations by noncontact atomic force microscopy (nc-AFM and Kelvin probe force microscopy (KPFM. With the aim to probe the photo-induced charge carrier generation, thin films deposited on transparent indium tin oxide substrates are investigated in dark conditions and upon illumination. The topographic and contact potential difference (CPD images taken under dark conditions are analysed in view of the results of complementary transmission electron microscopy (TEM experiments. After in situ annealing, it is shown that the dyads with longer donor blocks essentially lead to standing acceptor–donor lamellae, where the acceptor and donor groups are π-stacked in an edge-on configuration. The existence of strong CPD and surface photo-voltage (SPV contrasts shows that structural variations occur within the bulk of the edge-on stacks. SPV images with a very high lateral resolution are achieved, which allows for the resolution of local photo-charging contrasts at the scale of single edge-on lamella. This work paves the way for local investigations of the optoelectronic properties of donor–acceptor supramolecular architectures down to the elementary building block level.

  3. Estimation of residual stress in cold rolled iron-disks from strain measurements on the high resolution Fourier diffractometer

    International Nuclear Information System (INIS)

    Aksenov, V.L.; Balagurov, A.M.; Taran, Yu.V.

    1995-01-01

    The results of estimating residual stresses in cold rolled iron disks by measurements with the high resolution Fourier diffractometer (HRFD) at the IBR-2 pulsed reactor are presented. These measurements were made for calibration of magnetic and ultrasonic measurements carried out at the Fraunhofer-Institute for Nondestructive Testing in Saarbrucken (Germany). The tested objects were cold rolled steel disks of 2.5 mm thickness and diameter of about 500 mm used for forming small, gas pressure tanks. Neutron diffraction experiments were carried out at the scattering angle 2θ=+152 d eg with resolution Δd/d=1.5·10 -3 . The gauge volume was chosen according to the magnetic measurements lateral resolution 20x20 mm 2 . In the nearest future the neutron diffraction measurements with cold rolled iron disks at the scattering angle 2θ=±90 0 are planned. Also the texture analysis will be included in the Rietveld refinement procedure for more correct calculation of residual stress fields in the cold rolled materials. 8 refs., 10 figs., 1 tab

  4. C:\\Users\\AISA\\Desktop\\SILUE S..xps

    African Journals Online (AJOL)

    AISA

    in vitro, dépend en grande partie des génotypes ... NI : numéros d'introduction de la collection du Jardin Botanique National de Belgique (BE-1860 Meise), G et BAT ..... d'obtenir environ 69 % de fécondation 2 heures ... Statistique théorique et.

  5. C:\\Users\\AISA\\Desktop\\FOFANA INZA.xps

    African Journals Online (AJOL)

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    objectif est d'évaluer la variabilité de certains descripteurs afin d'identifier les plus discriminants .... permis d'évaluer les performances biométriques des populations. Les Analyses en Composantes. Principales (ACP) ont été conduites à l'aide du.

  6. XPS study of vanadium surface oxidation by oxygen ion bombardment

    Czech Academy of Sciences Publication Activity Database

    Alov, N.; Kutsko, D.; Spirovová, Ilona; Bastl, Zdeněk

    2006-01-01

    Roč. 600, č. 8 (2006), s. 1628-1631 ISSN 0039-6028 R&D Projects: GA ČR GA104/04/0467 Institutional research plan: CEZ:AV0Z40400503 Keywords : vanadium oxide * oxide film * ion-beam oxidation * X-ray photoelectron spectroscopy Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.880, year: 2006

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    African Journals Online (AJOL)

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    3Zootechnicien, Maître de Recherches Institut de l'Environnement et de Recherches Agricoles (INERA) 04 BP 8645 ... et sociales, mais aussi pour la génération .... METHODOLOGIE. Les poussins non sexés ont été transférés dans le poulailler au fur et à mesure de l'éclosion où ils ont été élevés durant trois semaines.

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    African Journals Online (AJOL)

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    1Ecole Inter-Etats des sciences et medecine Vétérinaires (EISMV) BP 5077 Dakar Sénégal. E-mail : diopthiouba@yahoo. ... pour la recherche du bois et 2 h pour la cuisson d'un repas contre (67,25 %) de ménages sans biodigesteurs qui y consacraient 2 à 6 h par .... Cette méthode consiste à mener une étude comparative ...

  9. C:\\Users\\AISA\\Desktop\\MBETID BESSANE.xps

    African Journals Online (AJOL)

    AISA

    , Laboratoire d'Economie Rurale ... le souci de sécurité et d'intégration sociale. .... METHODOLOGIE. APPROCHES THEORIQUE ET. CONCEPTUELLE. La reconversion est la réadaptation à des conditions nouvelles, qui impliquent le dévelop ...

  10. H:\\PMKER 25(3)\\TRAORE K..xps

    African Journals Online (AJOL)

    AISA

    Laboratoire de Phytopathologie de la Faculté d'Agronomie de l'Université de Parakou (Bénin) pour confirmer ou non la présence des trois virus responsables de maladies chez les Solanaceae à savoir le CMV, le PVMV et le PVYN. Des tampons ont été préparés conformément aux directives de Clarck et al. (1977), il s'agit.

  11. XPS studies of short pulse laser interaction with copper

    International Nuclear Information System (INIS)

    Stefanov, P.; Minkovski, N.; Balchev, I.; Avramova, I.; Sabotinov, N.; Marinova, Ts.

    2006-01-01

    The effect of laser ablation on copper foil irradiated by a short 30 ns laser pulse was investigated by X-ray photoelectron spectroscopy. The laser fluence was varied from 8 to 16.5 J/cm 2 and the velocity of the laser beam from 10 to 100 mm/s. This range of laser fluence is characterized by a different intensity of laser ablation. The experiments were done in two kinds of ambient atmosphere: air and argon jet gas. The chemical state and composition of the irradiated copper surface were determined using the modified Auger parameter (α') and O/Cu intensity ratio. The ablation atmosphere was found to influence the size and chemical state of the copper particles deposited from the vapor plume. During irradiation in air atmosphere the copper nanoparticles react with oxygen and water vapor from the air and are deposited in the form of a CuO and Cu(OH) 2 thin film. In argon atmosphere the processed copper surface is oxidized after exposure to air

  12. C:\\Users\\AISA\\Desktop\\S. TRAORE.xps

    African Journals Online (AJOL)

    AISA

    été appliqués, à des périodes imposées par le niveau d'enherbement de la parcelle. « La cercosporiose » a été contrôlée par des ablations mécaniques des feuilles nécrosées. Une semaine après plantation, chaque plant a reçu 100 g de dolomie (CaMg(CO3)2), et 100 g six mois après le premier apport. Le phosphate.

  13. H:\\PMKER 25(3)\\EGAH J..xps

    African Journals Online (AJOL)

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    de réponses ne favorisent que certaines variétés, laissant presqu'entière la question de la conservation de la biodiversité .... biodiversité de l'igname surtout que son système semencier en ...... framework for valuing on-farm genetic resources.

  14. C:\\Users\\AISA\\Desktop\\DSJC GBEMAVO.xps

    African Journals Online (AJOL)

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    l'impact de la variabilité des paramètres climatiques sur J. curcas, (ii) d'établir une équation de ... le contexte actuel de crise des combustibles .... Environment study and phytodistricts distribution. ..... fuel production, and socio-economic.

  15. H:\\PMKER 25(3)\\ZEZE A..xps

    African Journals Online (AJOL)

    AISA

    préalablement stérilisé à l'autoclave (110 °C,. 2 kg/cm2, 3h) et 150 g de sol de chaque échantillon servant d'inoculum (2 plants par pot). Après 75 jours de culture, 50 g de sols de chaque échantillon séché à l'air libre est utilisé pour extraire les spores selon la méthode de tamisage humide (Gerdemann et Nicolson,. 1963).

  16. C__Users_HP Pro 2000_Desktop_MOUNDZEO.xps

    African Journals Online (AJOL)

    HP Pro 2000

    P + RU. L'ETP a été calculée à partir de la formule de. Penman, très adaptée en milieu tropical humide. (Riou, 1975 ; Samba et Mbaye-Diop, 2000) comme suit : Où , est la pente de la courbe de la tension de vapeur saturante en fonction de la température de l'air, la constante psychrométrique (0,66 au niveau de la mer).

  17. C:\\Users\\AISA\\Desktop\\C. S. TRABI.xps

    African Journals Online (AJOL)

    AISA

    Besides the quality of the litter in connection with the composition of the food group of termites has been demonstrated by the presence of the species of ... the conservation of biodiversity depending on the time of the rest of these soils.

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    African Journals Online (AJOL)

    AISA

    nodules and permitted the application of the herbicide, better development of soybean plants. Herbicide ... négative sur les micro-organismes du sol, en particulier, sur les .... différences significatives entre les traitements sont apparus à partir de 45e jour après le semis. (JAS), et ce, jusqu'au 90e JAS. En effet, pendant ...

  19. H:\\PMKER 25(3)\\NOUATIN G..xps

    African Journals Online (AJOL)

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    Les institutions de micro finance, de part leur importance dans la réduction de la pauvreté dans les pays en développement, sont de plus en plus au centre des préoccupations aussi bien des politiques que des scientifiques. Au Bénin on compte ... En effet, il existe relativement peu d'analyses d'impact de programmes de ...

  20. C:\\Users\\AISA\\Desktop\\KOUASSI ROLAND.xps

    African Journals Online (AJOL)

    AISA

    grouping to Afrotrilepis pilosa and Sanseviera liberica. The objective of this study was to characterize the vegetable diversity of the grouping by floristic composition, biological and phytogeographical analysis. The study of the biological spectra highlighted the abundance and the predominance of the thérophytes and the.

  1. C:\\Users\\AISA\\Desktop\\K. KAMOU.xps

    African Journals Online (AJOL)

    AISA

    Diversity and Molecular phylogeny of the genus Lactifluus (Basidiomycota,. Russulales) in West Africa including new taxa. XXth Congress of AETFAT,. Stellenbosch (South Africa), 13th to 17th. January 2014, Scripta Botanica Belgica vol. 52: 251. Maba D. L., Guelly A. K., Yorou N. S., Agerer R. 2014 c. Progress in molecular ...

  2. C:\\Users\\AISA\\Desktop\\SORO S..xps

    African Journals Online (AJOL)

    AISA

    Propriétés insecticides et fertilisantes de l'engrais organique liquide «Ergofito Defense». ETUDE DE ... results were analyzed using the SAS software version 8.2. At 75 days after ... Par exemple, l'efficacité d'extraits de feuilles de neem.

  3. C:\\Users\\AISA\\Desktop\\KOUTOU A..xps

    African Journals Online (AJOL)

    AISA

    results indicate that Deli x La Mé Plant material from the first cycle of RRS displays an iodine index of 55. The values of oil iodine indices of trees from the second cycle of RRS showan improvement of 2 points for trees derived from crosses using DA5D x DA3D and DA115D AF as female parents (mean iodine index = 57).

  4. C:\\Users\\AISA\\Desktop\\M. CAMARA.xps

    African Journals Online (AJOL)

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    plus rapidement le capital investi dans l'établissement de la ... hydriques conduisent à l'arrêt de croissance puis à la mort des .... les plans humain et financier, afin de mieux cibler les actions de ... Rentabilité économique des techniques.

  5. Quantitative analysis of overlapping XPS peaks by spectrum reconstruction

    DEFF Research Database (Denmark)

    Graat, Peter C.J.; Somers, Marcel A. J.

    1998-01-01

    parameters. The values obtained for the oxide film thickness were compared with thickness values determined from the intensity of the corresponding O 1s spectra and with thickness values resulting from ellipsometric analysis. The sensitivity of the reconstruction procedure with regard to film thickness...... contributions in the spectra owing to inelastic scattering of signal electrons were calculated from the depth distributions of these constituents and their reference spectra. In the reconstruction procedure the film thickness and the concentrations of Fe/sup 2+/ and Fe/sup 3+/ in the oxide film were used as fit...

  6. C:\\Users\\AISA\\Desktop\\KALLEL SADREDDINE.xps

    African Journals Online (AJOL)

    AISA

    dans des récipients en plastique avec un couvercle de 12 cm de hauteur et présentant une base circulaire de 11cm de diamètre. Les sols sont par la suite humidifiés et déposés sur un papier filtre de 13 cm de diamètre préalablement humidifié et recevant soit des œufs de criquets soit des chenilles de Galleria mellonella.

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    African Journals Online (AJOL)

    AISA

    ordinateur. Au cours de ces dictées d'enregistrement de compor- tement et pour chaque femelle, sept paramètres ont été relevés et enregistrés à l'ordinateur : - durée de marche sans balayage (en sec) : pendant laquelle la femelle se déplace sur les.

  8. C:\\Users\\AISA\\Desktop\\SILUE N..xps

    African Journals Online (AJOL)

    AISA

    sèche, elle est réduite à l'état de paille sur pied lorsqu'elle n'est pas consumée par les feux de brousse (Koumi et ... forêts claires et des forêts galeries (Jourda et al., 2006). On rencontre également de nombreuses plantations ... informelles ont eu lieu avec les Responsables des dits villages. Le but de ces rencontres était.

  9. C:\\Users\\AISA\\Desktop\\BLE C.M..xps

    African Journals Online (AJOL)

    AISA

    Impact des pesticides agricoles et performances physiologiques des poissons ... du plasma en K+, en Cl- et en P a significativement baissé au fur et à mesure que la dose d' ... significantly increased (p < 0.05) in fish exposed to TIHAN (T2 group) than the control group (T0). ..... meilleure gestion de ces polluants dans les.

  10. C__Users_HP Pro 2000_Desktop_NUAMA.xps

    African Journals Online (AJOL)

    HP Pro 2000

    UFR de Sciences Economiques et de Gestion (Université de Cocody) / CIRES. 08 BP 1295 Abidjan 08. .... dégager une seule mesure de la productivité qui ... facteurs, qui échappent au contrôle des exploitants tels .... scores de performance.

  11. C:\\Users\\AISA\\Desktop\\F-G. GACHA.xps

    African Journals Online (AJOL)

    AISA

    Déterminants des conflits entre agriculteurs Baoulé et éleveurs peulh. ... agriculteurs et éleveurs subsistent, allant jusqu'à des affrontements .... rien n'est prévu par la loi ivoirienne pour .... plaignent de l'utilisation de bouviers mineurs qui.

  12. C:\\Users\\AISA\\Desktop\\B. DIALLO.xps

    African Journals Online (AJOL)

    AISA

    Pistacia vera L.). Comptes Rendus Biologies. Volume 332 ; (8) : 752 - 758. Borg P., Lê G., Lebrun S., Pées B. 2009. Example of industrial valorisation of derivative products of Castor oil. Innovation-. Technologie. Oléagineux, Corps Gras,. Lipides. Vol.

  13. C:\\Users\\AISA\\Desktop\\J. AVAKOUDJO.xps

    African Journals Online (AJOL)

    AISA

    du sol, la granulométrie, le taux de carbone organique du sol, l'azote total, les phosphores assimilable et total, la somme des bases échangeables ... la couverture végétale, la valeur d'agrément. (pression à l'emploi) et de gestion des terres ; ...... Changes to Physicochemical Properties of Ultisols Distributed on Calcareous.

  14. C__Users_HP Pro 2000_Desktop_DAKUO.xps

    African Journals Online (AJOL)

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    Effet du «compost plus» sur le compostage des tiges de cotonnier. EFFET DE ... et Systèmes de Production. RESUME .... systèmes de cultures qui repose sur une gestion rationnelle de la ..... Le respect des recommandations par les paysans ...

  15. H:\\PMKER 25(3)\\HALA.xps

    African Journals Online (AJOL)

    AISA

    plus fréquemment utilisées contre les cochenilles appartiennent au groupe des organophosphorés. Le chlorpyrifos-éthyl a montré une bonne efficacité comparativement aux pyréthrinoïdes tels que la bifenthrine et la lamdacyhalothrine (Dembélé, 2001). Toutes les formulations à base de chlorpyriphos- éthyl (Dursban 4 E, ...

  16. C:\\Users\\AISA\\Desktop\\TIECOURA K..xps

    African Journals Online (AJOL)

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    APEX CAULINAIRE DE MIL (Pennisetum glaucum (L.) R.) K. TIECOURA1, A. B. KOUASSI1, O. N'NAN-ALLA1, M. DINANT2 et L. LEDOU2. 1Laboratoire de Génétique, UFR Biosciences, Université Félix HOUPHOUËT-BOIGNY, 22 BP 582 Abidjan ...

  17. Mastering high resolution tip-enhanced Raman spectroscopy: towards a shift of perception.

    Science.gov (United States)

    Richard-Lacroix, Marie; Zhang, Yao; Dong, Zhenchao; Deckert, Volker

    2017-07-03

    Recent years have seen tremendous improvement of our understanding of high resolution reachable in TERS experiments, forcing us to re-evaluate our understanding of the intrinsic limits of this field, but also exposing several inconsistencies. On the one hand, more and more recent experimental results have provided us with clear indications of spatial resolutions down to a few nanometres or even on the subnanometre scale. Moreover, lessons learned from recent theoretical investigations clearly support such high resolutions, and vice versa the obvious theoretical impossibility to evade high resolution from a purely plasmonic point of view. On the other hand, most of the published TERS results still, to date, claim a resolution on the order of tens of nanometres that would be somehow limited by the tip apex, a statement well accepted for the past 2 decades. Overall, this now leads the field to a fundamental question: how can this divergence be justified? The answer to this question brings up an equally critical one: how can this gap be bridged? This review aims at raising a fundamental discussion related to the resolution limits of tip-enhanced Raman spectroscopy, at revisiting our comprehension of the factors limiting it both from a theoretical and an experimental point of view and at providing indications on how to move the field ahead. It is our belief that a much deeper understanding of the real accessible lateral resolution in TERS and the practical factors that limit them will simultaneously help us to fully explore the potential of this technique for studying nanoscale features in organic, inorganic and biological systems, and also to improve both the reproducibility and the accuracy of routine TERS studies. A significant improvement of our comprehension of the accessible resolution in TERS is thus critical for a broad audience, even in certain contexts where high resolution TERS is not the desired outcome.

  18. Sulfurized activated carbon for high energy density supercapacitors

    Science.gov (United States)

    Huang, Yunxia; Candelaria, Stephanie L.; Li, Yanwei; Li, Zhimin; Tian, Jianjun; Zhang, Lili; Cao, Guozhong

    2014-04-01

    Sulfurized activated carbon (SAC), made by coating the pore surface with thiophenic sulfur functional groups from the pyrolysis of sulfur flakes, were characterized and tested for supercapacitor applications. From X-ray photoelectron spectroscopy (XPS), the sulfur content in the SAC was found to be 2.7 at%. Electrochemical properties from potentiostatic and galvanostatic measurements, and electrochemical impedance spectroscopy (EIS) were used to evaluate the effect of sulfur on porous carbon electrodes. The SAC electrode exhibits better conductivity, and an obvious increase in specific capacitance that is almost 40% higher than plain activated carbons (ACs) electrode at a high current density of 1.4 A g-1. The proposed mechanism for improved conductivity and capacitive performance due to the sulfur functional groups on ACs will be discussed.

  19. Study on the surface sulfidization behavior of smithsonite at high temperature

    Science.gov (United States)

    Lv, Jin-fang; Tong, Xiong; Zheng, Yong-xing; Xie, Xian; Wang, Cong-bing

    2018-04-01

    Surface sulfidization behavior of smithsonite at high temperature was investigated by X-ray powder diffractometer (XRD) along with thermodynamic calculation, X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA). The XRD and thermodynamic analyses indicated that the smithsonite was decomposed into zincite at high temperatures. After introducing a small amount of pyrite, artificial sulfides were formed at surface of the obtained zincite. The XPS analyses revealed that the sulfide species including zinc sulfide and zinc disulfide were generated at the zincite surface. The EPMA analyses demonstrated that the film of sulfides was unevenly distributed at the zincite surface. The average concentration of elemental sulfur at the sample surface increased with increasing of pyrite dosage. A suitable mole ratio of FeS2 to ZnCO3 for the surface thermal modification was determined to be about 0.3. These findings can provide theoretical support for improving the process during which the zinc recovery from refractory zinc oxide ores is achieved by xanthate flotation.

  20. Stacking it up: Exploring the limits of ultra-high resolution atomic force microscopy

    NARCIS (Netherlands)

    van der Heijden, N.J.

    2017-01-01

    Atomic force microscopy (AFM) is a technique wherein an atomically sharp needle raster scans across a surface, detecting forces between it and the sample. In state-of-the-art AFM experiments the measured forces are typically on the order of pico-Newtons, and the lateral resolution is on the order of