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  • Articles  (79)
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  • 1
    Electronic Resource
    Electronic Resource
    Boron Carbonitride Thin Films by PACVD of Single-Source PrecursorsWe thank Prof. U. Klingebiel, University of Göttingen, for providing the TBBD, Dr. R. Rein, Institut für Neue Materialien, Saarbrücken, for the hardness measurements, and Dr. H.-J. Kleebe, Universität Bayreuth, Institut für Materialforschung, for the TEM analysis. (1997)
    Weinheim : Wiley-Blackwell
    Chemical Vapor Deposition 3 (1997), S. 257-262 
    Details
    ISSN: 0948-1907
    Keywords: Boron carbonitride ; PACVD ; Pyridine-borane ; AES ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: This work investigates the influence of the carrier gases N2, Ar, and He and the influence of the applied power density (about 1-4 W/cm2) on the chemical composition of boron carbonitride films deposited by a PACVD process. The plasma is activated via 13.56 MHz radio frequency. Si(100) wafers were used as substrates and pyridine-borane (PB) and triazaborabicyclodecane (TBBD) as B-C-N-forming single-source precursors. Films that were either deposited in He using a low power density or in N2 using a high power density showed comparable properties. Analysis of these films showed their chemical composition to be BC4N. Moreover, they exhibited outstanding hardnesses of up to 64 GPa. A simple model describing the acceleration of B, C, and N ions in the plasma towards the substrate showed comparable ion momenta by use of the corresponding deposition parameters. Basically, it was found that, the higher the ion momentum, the higher the film hardness.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cvde.19970030503
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  • 2
    Electronic Resource
    Electronic Resource
    Chemical states of iodine in iodine-doped polystyrene (1996)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 34 (1996), S. 587-590 
    Details
    ISSN: 0887-6266
    Keywords: iodine-doped polystyrene ; charge-transfer (CT) complex ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: No abstract.
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  • 3
    Electronic Resource
    Electronic Resource
    Structure-conductivity relationships of iodine-doped polyaniline (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 1993-2001 
    Details
    ISSN: 0887-6266
    Keywords: polyaniline ; conducting polymer ; iodine doping ; XPS ; FTIR ; TGA ; WAXD ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyaniline, synthesized by using potassium dichromate as the oxidant, was doped with iodine in order to increase its electrical conductivity. The iodine-doped polyanilines attained a conductivity of 1.83 × 10-3 S/cm, which was about eight orders of magnitude greater than that of intrinsic polyaniline. The iodine-doped polyanilines did not absorb moisture readily when compared to the protonic-acid-doped polyanilines. Fourier transform infrared (FTIR) and x-ray photoelectron spectroscopy (XPS) results indicated that iodine-doping reactions occurred at the N-atoms in the quinoid structural units of the polyaniline molecular chains and consequently formed the charge transfer complexes. The iodine in the iodine-doped polyanilines existed mainly in the forms of I-3 and I-5 anions. As the doping level increased, the relative content of I-5 anions increased. Thermogravimetric analysis (TGA) results showed that there was about 6 wt % of iodine strongly bonded to the polyanilines since they would not evolve even at the structural decomposition temperatures of the polymer backbones. Wide-angle x-ray diffraction spectroscopy (WAXD) results revealed that the intrinsic polyaniline was an amorphous polymer but the regularity of polyaniline chains increased after iodine-doping. The iodine-doped polyanilines also showed a decrease in thermal stability. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 1993-2001, 1997
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  • 4
    Electronic Resource
    Electronic Resource
    X-ray photoelectron spectroscopic studies of charge transfer interactions in electroactive polyaniline (1994)
    New York, NY : Wiley-Blackwell
    Polymers for Advanced Technologies 5 (1994), S. 171-177 
    Details
    ISSN: 1042-7147
    Keywords: Polyaniline ; XPS ; Charge transfer ; Oxidation states ; Films ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Four modes of charge transfer interactions in polyaniline (PAN), viz. acid protonation, self-doping, charge transfer interactions with organic acceptors, and charge transfer interactions with surface grafted functional polymers have been studied by X-ray photoelectron spectroscopy (XPS). In the case of acid protonation, the protonation behavior of volatile and non-volatile acid differs. The structures of sulfonated leucomeraldine (LM) and nigraniline (NA) are similar to those of sulfonated and self-protonated emeraldine (EM). A substantially higher degree of charge transfer interaction with the organic acceptors is observed for EM film that has been subjected to one cycle of acid/base treatment. The charge transfer interactions with the organic acceptors have proceeded further than the pure formation of molecular complexes. Both pristine and Ar plasma or O3 pretreated EM films are susceptible to surface modifications by graft copolymerization. The protonic acid functional groups of the graft readily give rise to a self-protonated EM surface.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/pat.1994.220050305
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  • 5
    Electronic Resource
    Electronic Resource
    Surface structures of fluoropolymer, polyolefin and polyester films after modification by graft polymerization (1994)
    New York, NY : Wiley-Blackwell
    Polymers for Advanced Technologies 5 (1994), S. 837-842 
    Details
    ISSN: 1042-7147
    Keywords: Polyolefin ; Fluoropolymer ; Polyester ; Graft Polymerization ; Surface structure ; XPS ; SIMS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Pristine and argon plasma pretreated polytetrafluoroethylene (PTFE), polystyrene (PS), high-density polyethylene (HDPE) and poly(ethylene terrephthalate) (PET) films have been subjected to near-UV light-induced graft polymerization with water-soluble acrylamide (AAm), the sodium salt of styrene sulfonic acid (NaSS), acrylic acid (AAc) and N,N-dimethylaminoethylmethylacrylate (DMAEMA) monomers. The structure and composition at the substrate surface with grafted polymer were studied by angle-resolved X-ray photoelectron spectroscopy (XPS). In most cases, the density of surface grafting is enhanced by plasma pretreatment. For each polymer substrate with a substantial amount of grafting, the hydrophilic graft penetrates or becomes partially submerged beneath a thin surface layer of dense substrate chains. This stratified microstructure is consistent with the static secondary ion mass spectroscopy (SIMS) and Ar+ beam depth profiling results. The two latter techniques also suggest that when the grafted polymer has a bulky substituent, there is less efficient penetration of the grafted polymer below the surface.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/pat.1994.220051211
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  • 6
    Electronic Resource
    Electronic Resource
    Surface analytical techniques (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Advanced Materials for Optics and Electronics 5 (1995), S. 53-70 
    Details
    ISSN: 1057-9257
    Keywords: AES ; XPS ; SIMS ; SNMS ; laser Raman microscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: This review briefly describes some of the techniques available for analysing surfaces and illustrates their usefulness with a few examples. In particular, Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), secondary ion mass spectroscopy (SIMS), sputter neutral mass spectroscopy (SNMS) and laser Raman spectroscopy are all described. 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. SIMS and SNMS can be performed together and can detect smaller surface concentrations. Laser Raman spectroscopy is useful for determining molecular bonding. Techniques which give topographic information, such as scanning tunnelling microscopy (STM) and atomic force microscopy (AFM), have not been considered.
    Additional Material: 18 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/amo.860050202
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  • 7
    Electronic Resource
    Electronic Resource
    Surface properties and drug release behavior of polycaprolactone polyether blend and copolymer (1996)
    New York, NY : Wiley-Blackwell
    Polymers for Advanced Technologies 7 (1996), S. 104-107 
    Details
    ISSN: 1042-7147
    Keywords: polycaprolactone-poly(ethylene glycol) block copolymer ; blended polymer ; XPS ; surface property ; drug release behavior ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: The surface properties of polycaprolactone (PCL)-poly(ethylene glycol) (PEG) block copolymer (PCE) and blend (B-PCE) of PCL and PEG obviously affect the drug release behavior of the polymer. In this paper, both surface properties of PCE and B-PCE are studied and compared by measuring their water sorption and using the contact angle and X-ray photoelectron spectroscopy technique. The effect of the polyether segment content in PCE and B-PCE on hydrophilicity is discussed. The results show that a hydrophilic polyether segment moves towards the surface and enriches on the surface for either PCE or B-PCE. The enrichment content of the polyether segment of PCE and the hydrophilicity of its surface are higher than that of B-PCE. A reason for the different drug release rates for PCE and B-PCE is suggested.
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  • 8
    Electronic Resource
    Electronic Resource
    A Study of the Chemical Bonding and Microstructure of Ion Beam-deposited CNx Films Including an XPS C 1s Peak Simulation (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 629-642 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; FTIR ; carbon nitride ; thin film ; simulation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The chemical bonding and microstructure of dual ion beam-deposited CNx films with nitrogen contents in the range 20-33 at.% have been examined by Fourier transform infrared spectroscopy (FTIR) and x-ray photoelectron spectroscopy (XPS). The FTIR spectra together with other published data have been used to construct a model microstructure of the CNx films. The XPS N 1s peak is composed of two components corresponding to N-sp2 C and N-sp3 C bonds. Using the quantified N 1s data and making certain assumptions, the model microstructure has been used as the basis of a C 1s peak simulation in which nine C components have been combined. At an N content of 20 at.% the simulation agrees well with the experimentally recorded XPS C 1s peak. The FTIR spectra, XPS N 1s peak shape and C 1s peak simulations support a microstructure of N substitution into an amorphous sp2/sp3 hybridized carbon structure. Above an N content of ∽20%, a new (nitrile-like) chemical form also emerges in the material, its abundance increasing with N content. It is proposed that this new structure occurs due to the presence, in the surface region of the condensing film, of C≡N dimers, which are formed when a C atom is surrounded by many N atoms. This molecule becomes trapped in the material and bonds to atoms at neighbouring sites. © 1997 by John Wiley & Sons, Ltd.
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  • 9
    Electronic Resource
    Electronic Resource
    Study of the Chemical Composition and Microstructure of Ion Beam-deposited CNx Films Including an XPS C 1s Peak Simulation (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 301-314 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; FTIR ; carbon nitride ; thin film ; simulation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The chemical composition and microstructure of dual ion beam-deposited CNx films with nitrogen contents in the range 20-33 at.% have been examined by Fourier transform infrared spectroscopy (FTIR) and x-ray photoelectron spectroscopy (XPS). The FTIR spectra together with other published data have been used to construct a model microstructure of the CNx films. The XPS N 1s peak is composed of two components corresponding to N-sp2 C and N-sp3 C bonds. Using the quantified N 1s data and making certain assumptions, the model microstructure has been used as the basis of a C 1s peak simulation in which nine C components have been combined. At an N content of 20 at.% the simulation agrees well with the experimentally recorded XPS C 1s peak. The FTIR spectra, XPS N 1s peak shape and C 1s peak simulations support a chemical structure of N substitution in an amorphous sp2/sp3 hybridized carbon structure. Above an N content of ∽20%, a new (nitrile-like) chemical form also emerges in the material, its abundance increasing with N content. It is proposed that this new structure occurs due to the presence, in the surface region of the condensing film, of C—N dimers, which are formed when a C atom is surrounded by many N atoms. This molecule becomes trapped in the material and bonds to atoms at neighbouring sites. © 1997 John Wiley & Sons, Ltd.
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  • 10
    Electronic Resource
    Electronic Resource
    XPS, XANES and ToF-SIMS Characterization of Reactively Magnetron-sputtered Carbon Nitride FilmsPresented at ECASIA '95 Montreux, Switzerland, October 1995. (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 315-323 
    Details
    ISSN: 0142-2421
    Keywords: carbon nitride ; PVD ; hybridization ; AES ; XPS ; XANES ; ToF-SIMS ; magnetron-sputtered film ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The existence of β-C3N4 with hardness characteristics similar or better than diamond was predicted in 1990 by Liu and Cohen. Many studies have since been devoted to the synthesis of this compound. In the present work, carbon nitride films were deposited by various reactive magnetron sputtering processes of graphite targets in pure nitrogen and characterized by AES, XPS, x-ray adsorption near-edge structure (XANES) and static time-of-flight SIMS (ToF-SIMS). Various bonding states (single and double bond) are observed between carbon and nitrogen atoms and between carbon atoms but there is no evidence in the XANES results for either the presence of carbon-nitrogen triple bonds or a pyridine-like ring structure. Surface N/C ratios were estimated to be close to 0.3. Carbon K-edge XANES lineshapes, the C 1s plasmon-loss structure and the calculated density (2.2 g cm-3) indicate that the films are similar to diamond-like carbon without long-range ordering. The presence of CxNy fragments with 1≤y〈4 and the low abundance of CHx and CHxNy fragments in ToF-SIMS spectra further confirm that the carbon atoms do not adopt a graphite or pyridine-like cyclic two-dimensional structure and that the films are not significantly hydrogenated. A three-phase solid solution model is proposed for the composition of the films: a ‘free’ carbon phase, an sp3 - carbon-nitrided phase and an sp2 - carbon-nitrided phase. The relative proportion of these phases is influenced by the deposition conditions. Enhanced plasma ionization reactive magnetron sputtering leads to higher density and to a higher fraction of the sp3 carbon phase. © 1997 John Wiley & Sons, Ltd.
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  • 11
    Electronic Resource
    Electronic Resource
    Incorporation of Surface Topography in the XPS Analysis of Curved or Rough Samples Covered by Thin Multilayers (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 741-746 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; coating thickness ; global analysis ; multilayers ; curvature ; roughness ; atomic force microscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Approaches are described for the analysis of XPS signals from samples comprising thin conformal coatings on substrates with non-ideal surface topography. In particular, attention is focused on arbitrarily shaped rough or curved substrates. Relations are derived for the relative x-ray photoelectron intensities emitted from various elements in such non-ideal samples. The surface topography of arbitrarily rough samples is analysed by atomic force microscopy to provide a frequency histogram of the local slopes, which is incorporated into a global, multi-element analysis method for interpretation of the observed XPS elemental intensities. An analogous approach is used for the analysis of curved samples. Our algorithms also enable simultaneous analysis of successively coated multilayer structures. When the elemental composition of the individual layers is known, the fit procedure enables determination of the thickness values of single-layer and multilayer coatings. The range of validity of the theory is discussed. © 1997 by John Wiley & Sons, Ltd.
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  • 12
    Electronic Resource
    Electronic Resource
    XPS Studies of Oxide Growth and Segregation in Aluminium-Silicon Alloys (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 809-816 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; Al-Si alloy ; segregation ; oxide growth ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The oxidation of three aluminium-silicon alloys has been studied as a function of temperature. At temperatures below 473 K a thin passivating oxide film is formed. At higher temperatures the segregation of the trace element magnesium to the surface is observed where it dominates the subsequent oxidation behaviour. In the absence of oxygen, magnesium segregation does not occur. From these results it is concluded that at temperatures in excess of 473 K magnesium segregation controls oxide growth and also that the degree of segregation is temperature dependent. Segregation effects are also observed for sodium, which appears to be concentration limited, and silicon, which is confined to the alumina-rich regions close to the metal surface where the silicon is also oxidized. © 1997 by John Wiley & Sons, Ltd.
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  • 13
    Electronic Resource
    Electronic Resource
    Control of the stoichiometry in the deposition of cobalt oxides on SiO2 (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 62-71 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; ISS ; CoO ; Co3O4 ; interface effects ; cobalt oxide ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Both CoO and Co3O4 overlayers have been deposited on SiO2 by evaporation from metallic Co and subsequent oxidation with oxygen and a plasma of oxygen. The combined use of ion scattering spectroscopy and XPS shows that both oxides grow in the form of small particles on the surface of SiO2. Ion scattering spectroscopy also shows that the surface of cobalt oxide exposed to a plasma of oxygen is enriched in oxygen ions with respect to the surface of the cobalt oxide formed by exposure to oxygen. The Co 2p spectra corresponding to the deposits obtained by oxidation with O2 are characteristic of CoO, while those corresponding to the deposits obtained after oxidation with a plasma are typical of Co3O4. Moreover, the OCo/Co ratios determined by XPS and factor analysis indicate the formation of CoO stoichiometry in the former case and Co3O4 stoichiometry in the latter. It has also been observed that no shift in either binding energy or modified Auger parameter α′ appears as a function of coverage. This absence of shifts is interpreted as a consequence of the type of screening mechanism that dominates the relaxation of the photoholes in these oxides. © 1998 John Wiley & Sons, Ltd.
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  • 14
    Electronic Resource
    Electronic Resource
    Initial adsorption of trimethylsilane on Ge(100) surfaces (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 113-120 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; Ge ; adsorption ; trimethylsilane ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Trimethylsilane (TMSiH) was adsorbed onto a Ge(100) surface at a temperature of -150±3°C and x-ray photoelectron spectroscopy (XPS) was used to study the resulting surface species as functions of the TMSiH exposure in Langmuir (L). The core-level C 1s, Si 2p and Ge 3d photoelectrons were monitored after each dosing. It was observed that the C-C bonds are the dominant species formed at the low doses of TMSiH. The second abundant species at the low coverage is the C-Ge bond. This indicated dissociative adsorption of TMSiH molecules onto a clean Ge(100) surface, which is similar to the adsorption of TMSiH molecules onto an Si(100) surface. As the dose increases, the Si-C species gradually increase due to physisorbed TMSiH on top of the C-C- and C-Ge-covered surface. This study clearly reveals the growth processes of TMSiH on a Ge(100) surface. The electronegativities of C, Si and Ge and the bond strengths of C-C, C-Si and C-Ge were invoked to discuss the initial formation of C-C and C-Ge on the Ge(100) surface. © 1998 John Wiley & Sons, Ltd.
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  • 15
    Electronic Resource
    Electronic Resource
    Identification of Mo(V) commonly observed in passive films formed on stainless steels (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 155-159 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; ESR ; electron spin resonance ; Mo 3d ; Mo 3p ; O 1s ; binding energies ; Mo(IV) ; Mo(V) ; Mo(VI) ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: There has been a longstanding debate and controversy in the literature with regard to the determination by XPS of the exact oxidation state of a molybdenum species commonly observed in the passive films of stainless steel. In this paper we have compared both the XPS and ESR analyses of molybdenum oxyhydroxides previously postulated to contain Mo(V) as well as Mo(IV) and Mo(VI). The compositions of these compounds closely resemble those found in the passive films of Mo-bearing stainless steel. It has been shown that the same Mo species exhibiting an XPS Mo 3d5/2 spectrum binding energy value of 230.8 eV is observed to exhibit an ESR spectra having a g factor of 1.921, which corresponds to Mo(V). © 1998 John Wiley & Sons, Ltd.
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  • 16
    Electronic Resource
    Electronic Resource
    Auger parameter determination of bonding states on thinly oxidized silicon nitride (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 134-143 
    Details
    ISSN: 0142-2421
    Keywords: Auger parameter ; silicon nitride ; x-ray photoelectron spectroscopy ; XPS ; Auger electron spectroscopy ; AES ; oxidation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Silicon nitride powders have been thermally oxidized between 700 and 1200°C in a high-purity N2-20% O2 gas environment. The powders were subsequently analyzed by x-ray photoelectron and Auger electron spectroscopies for evidence of oxynitride surface states. Measurements were made on the Si 2p, O 1s, N 1s, C 1s, F 1s and Si KLL transitions, the latter being obtained using bremsstrahlung radiation from the Mg x-ray source. As a function of increasing temperature the data show a clear progression of spectral binding energies and peak shapes that are indicative of more advanced surface oxidation. However, definitive analysis of these data rests on the combined use of both Auger and photoelectron data to define the oxidized surface states for a system that involves two electrically insulating end states: silicon nitride and silicon dioxide. Curve fitting the Si 2p and Si KLL transitions as a function of oxidation, coupled with the use of Auger parameters for the starting silicon nitride and final silicon dioxide, reveals no measurable evidence for an interphase oxynitride in the thin oxide scales of this study where the silicon nitride substrate is detectable. Possible incorrect assignment of oxynitride bonding, from shifted Si 2p states in the carbon referenced spectra, is attributable to band bending as the transition is made from incipient to fully formed silicon dioxide. © 1998 John Wiley & Sons, Ltd.
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  • 17
    Electronic Resource
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    Accuracy of the non-destructive surface nanostructure quantification technique based on analysis of the XPS or AES peak shape (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 249-269 
    Details
    ISSN: 0142-2421
    Keywords: quantitative surface analysis ; XPS ; AES ; nano-structures ; peak shape analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The accuracy of XPS and AES quantification by peak shape analysis was established from a detailed analysis of a range of model spectra and three sets of experiments. It was found that information on the concentration-depth profile in the surface region up to depths of ∽5λi (where λi is the inelastic electron mean free path) is primarily contained in the spectral energy region up to ∽100 eV below the peak energy and is essentially completely contained by the energy region up to ∽200 eV below the peak. Analysis of a larger energy range than 100 eV does not add much to the information on the details of the structure in the outermost 5λi but gives the possibility to determine additional structural parameters that describe the composition at larger depths. The structural parameters that describe the chemical composition of the outermost 5-10λi of the solid were divided into primary and secondary parameters: the primary parameters are the three most important parameters needed to describe the main characteristics of the distribution of atoms; the secondary parameters are parameters other than the three primary parameters that describe the finer details of the depth distribution of atoms in the outermost 5-10λi of the surface region. The uncertainty in the determined three primary parameters is typically 5-10%. The uncertainty in the determined secondary parameters is typically ≳35%. Different models of depth profiles can be distinguished when they differ significantly over a width of more than ∽1/3λi at any depth ≲5λi. The uncertainty in the total determined amounts of atoms within the surface region is ∽5-10% as long as the depths are within the primary probing depth of the method (i.e. 〈5λi). The absolute quantification of a set of samples where the in-depth distribution varies considerably gives a root-mean-square scatter of 15%. This is reduced to ∽10% when elastic scattering effects are modelled by a simple analytical expression. © 1998 John Wiley & Sons, Ltd.
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  • 18
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    High-resolution x-ray photoelectron spectroscopy of aliphatic hydrocarbons (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 278-289 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; aliphatic ; hydrocarbon ; high resolution ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Comparison of high-resolution core-level spectra from simple long-chain aliphatic hydrocarbons and hydrocarbon polymers show minor differences between ideal, specially prepared samples and samples of ‘as-received’ materials. Asymmetric peaks whose structure may be attributed to vibrational-level excitation can be resolved easily under conditions that do not cause damage. This asymmetric structure is independent of sample morphology and sampling depth. © 1998 John Wiley & Sons, Ltd.
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    Effect of RCA cleaning on the surface chemistry of glass and polysilicon films as studied by ToF-SIMS and XPS (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 270-277 
    Details
    ISSN: 0142-2421
    Keywords: RCA clean ; glass ; surface chemistry ; polysilicon ; thin film transistor ; ToF-SIMS ; XPS ; x-ray photoelectron spectroscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The surface chemistry of an alkaline-earth boroaluminosilicate glass is changed by contact with chemical solutions. The present study shows that RCA cleaning creates a silica-rich surface on the glass. This altered surface can be removed by hydrofluoric acid etching. During the RCA cleaning process, glass components can be transferred to a polysilicon film placed in the same alkaline solution. The acidic solution in turn removes most of the contamination from the polysilicon. © 1998 John Wiley & Sons, Ltd.
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    Surface charging of insulating samples in x-ray photoelectron spectroscopy (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 490-497 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; surface charging ; insulators ; organic overlayers ; differential charging ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Electrical charging of insulating samples during XPS is of direct concern for referencing the binding energy scale. Results are presented on charging of composite insulating samples that consist of an organic overlayer of polystyrene (PS) or polydimethylsiloxane (PDMS) deposited on NaCl particles. The samples were analysed using small-spot monochromatized radiation, the surface charge being stabilized with an electron flood gun. The charging shift of the NaCl substrate is influenced by three different factors: the total photoelectron flux, the energy of the electrons produced by the flood gun and the flux of electrons originating from the overlayer. The overlayer is acting as an additional electron source, which makes the substrate more negative and reduces inhomogeneities of the local potential affecting the peak full width at half-maximum. Comparison of substrate peak intensities with computed values showed that PS overlayers were less uniform compared to PDMS overlayers. The overlayer thickness and uniformity affect both the total photoelectron flux and the flux of electrons from the overlayer to the substrate. Overlayer charging, like substrate charging, is probably determined by the balance of electron fluxes in the phase considered. The kinetic energy of the photoelectron is determined by the electrical potential in the phase where photoemission occurs and not with respect to the sample surface. This was demonstrated by differential charging between the NaCl substrate and PS overlayer. © 1998 John Wiley & Sons, Ltd.
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    Resolution enhancement of x-ray photoelectron spectra by maximum entropy deconvolution (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 195-203 
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    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; deconvolution ; resolution ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The maximum entropy method (MEM) is applied to the deconvolution of x-ray photoelectron spectra. This method provides the least-biased estimate of the unbroadened spectrum by using the Shannon information content as the regularizing functional. The large-scale, non-linear optimization problem is solved using a robust variable metric sequential-quadratic programming (SQP) algorithm implemented on a personal computer (PC). The program is tested on simulated spectra and then shown to provide reliable resolution enhancement of measured spectra by unfolding a measured instrumental resolution function. Typical resolution enhancements of 50% are achievable in 〈15 min of computer time. © 1998 John Wiley & Sons, Ltd.
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    Oxidation of ternary TiZrN hard coatings studied by XPS (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 242-248 
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    ISSN: 0142-2421
    Keywords: hard coatings ; electrochemistry ; high temperature ; oxidation ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Electrochemical and thermal oxidation of TiZrN hard coatings deposited by the plasma beam sputtering technique are investigated using x-ray photoelectron spectroscopy (XPS). Ternary TiZrN coatings are found to be more susceptible towards oxidation compared to binary TiN and ZrN coatings. Electrochemical oxidation results in the formation of a mixed Ti(N,O)+Zr(N,O) oxynitride layer in the lower potential range (up to 1.1 V), whereas at higher potentials a mixed TiO2+ZrO2 oxide layer is formed. This layer still incorporates a certain amount of nitrogen released during transformation of nitride to oxide. A similar is observed in the case of thermal oxidation at 350-600°C, where the main product is a mixed TiO2+ZrO2 layer. Nitrogen, which should normally be evolved during oxidation, remains incorporated in the growing oxide layer. No tendency towards alternate layer formation, i.e. ZrO2/TiO2, was observed under the experimental conditions investigated. © 1998 John Wiley & Sons, Ltd.
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    Characterization of polyimide Langmuir-Blodgett films on silver using infrared, Raman and x-ray photoelectron spectroscopies (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 316-328 
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    ISSN: 0142-2421
    Keywords: IR ; infrared ; Raman ; XPS ; x-ray photoelectron spectroscopy ; polyimide ; Langmuir-Blodgett ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Ultrathin films of the dimethylhexadecylamine salt of the polyamic acid of pyromellitic dianhydride (PMDA) and oxydianiline (ODA) were deposited onto silver substrates using the Langmuir-Blodgett (LB) technique. These films were transformed to PMDA/ODA polyimide by both thermal and chemical processes. Reflection-absorption infrared spectroscopy (RAIR), surface-enhanced Raman scattering (SERS) and x-ray photoelectron spectroscopy (XPS) indicated that there was no strong interaction between the tertiary amine salt films and the silver substrates and that imidization of these films was quite complete. Both RAIR and SERS were also used to determine the molecular orientation in as-deposited tertiary amine salt films and in films that were imidized. It was concluded that ODA moieties were parallel to the silver surfaces in the as-deposited films. However, both SERS and RAIR indicated that imide formation induced orientation in which the PMDA moieties became more perpendicular to the silver surface while the ODA moieties were more parallel. © 1998 John Wiley & Sons, Ltd.
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    Catalytic combustion of methane: surface characterization of manganese-substituted barium hexa-aluminate catalysts (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 367-373 
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    ISSN: 0142-2421
    Keywords: methane ; catalytic combustion ; hexa-aluminate ; manganese ; LEEIXS ; XPS ; auger parameter ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: In order to achieve a good activity with respect to methane combustion, a good route would be via catalysts incorporating transition metals. For devices operating at high temperatures, such as gas turbines, substituted hexa-aluminates present the advantage of good thermal stability when compared to impregnated Al2O3. For the purpose of this study, manganese-substituted hexa-aluminates were prepared either by the sol-gel method or by carbonate precipitation. Surfaces were analysed by soft x-ray emission, namely low-energy electron-induced x-ray spectroscopy (LEEIXS), and by photoelectron spectroscopy, namely x-ray photoelectron spectroscopy. The results on samples incorporating increasing amounts of manganese show the existence of an upper limit to the number of atoms substituted at the catalyst surface. This limit is about 2.7 manganese ions per unit cell, for samples prepared either by the sol-gel or by the carbonate precipitation technique and then calcinated at 1200°C. The interpretation of the Auger parameter variations shows that the relative amount of Mn in oxidation state III increases when the surface amount of Mn increases, as well as with the Mn substitution level. This fact can be related to an increased activity for methane conversion. © 1998 John Wiley & Sons, Ltd.
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    Surface characterization of synthetic vulcanized rubber treated with oxygen plasma (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 385-399 
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    ISSN: 0142-2421
    Keywords: oxygen plasma ; surface treatment ; styrene-butadiene rubber ; adhesion ; T-peel strength ; XPS ; IR-ATR spectroscopy ; contact angle measurements ; SEM ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The surface of a synthetic vulcanized styrene-butadiene rubber (R2) was treated in an oxygen plasma to improve adhesion in joints prepared with a one-component solvent-based polyester-urethane adhesive. The modifications produced on the rubber surface by plasma treatment were assessed using advancing and receding contact angle measurements, x-ray photoelectron spectroscopy, (XPS), infrared-attenuated total reflection spectroscopy and scanning electron microscopy. Adhesion was obtained from T-peel tests of treated R2 rubber/polyurethane adhesive joints. Several experimental variables were considered, such as the radio-frequency power and the length and lifetime of the plasma treatment. The treatment in the oxygen plasma produced a noticeable decrease in contact angle, which can be mainly ascribed to the creation of C—O and C=O moieties on the rubber surface. Advancing and receding contact angles only differed by ∽10°. Depending on the experimental conditions used, some ablation was produced on the surface, which was more noticeable as the length and power of the treatment increased. An adequate performance of adhesive joints was obtained using a power of 50 W and a time for oxygen plasma treatment of 〈10 min. The changes in the rubber surface remained for 2 h after plasma treatment, as indicated by the variation in peel strength and XPS data. Although improved adhesion was obtained by treating the rubber in an oxygen plasma, the T-peel strength values are not sufficient to assure technical use, probably due to the migration of waxes and zinc stearate to the surface once the treatment was carried out. Finally, sulfur oxidation was produced by the plasma treatment, and for severe conditions solid crystals of a sodium salt of an oxidized sulfur compound (sodium sulphate or an organic sulphate) appeared on the treated rubber surface. © 1998 John Wiley & Sons, Ltd.
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    Part 1. N-(m-(3-(trifluoromethyl)diazirine-3-yl)phenyl)-4-maleimido-butyramide (MAD) on silicon, silicon nitride and diamond Dedicated to Professor Siegfried Hofmann on the occasion of his 60th birthday. (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 783-792 
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    ISSN: 0142-2421
    Keywords: ToF-SIMS ; XPS ; biomaterials ; biomolecules ; surface modification ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and x-ray photoelectron spectroscopy (XPS) are used to characterize the grafting of the reagent N-(m-(3-(trifluoromethyl)diazirine-3-yl)phenyl)-4-maleimido-butyramide (MAD) to various substrates: silicon, silicon nitride and diamond. MAD carries a maleimide function for thermochemical modification of thiolated molecules and a diazirine function that is lost during light activation (350 nm light). Photoactivation leads to carbene-mediated grafting to solid supports. X-ray photoelectron spectroscopy atomic constituents and chemical shifts, as well as ToF-SIMS molecular peaks and characteristic fragments of the photoimmobilized molecule, are identified. Extended interpretation of surface analysis data suggests that diamond is the substrate with the highest MAD grafting efficiency and that the formation of C-O bonds upon diazirine photoactivation is involved. The difference in grafting extent for the three substrates leads to the conclusion that other reaction sites could be involved but they are not identified. © 1998 John Wiley & Sons, Ltd.
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    Compositional changes in plasma-deposited fluorocarbon films during ageing (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 498-511 
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    ISSN: 0142-2421
    Keywords: plasma polymers ; fluorocarbons ; oxidation ; ageing ; surface restructuring ; XPS ; FTIR ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Plasma polymer coatings were deposited from perfluoro-1,3-dimethylcyclohexane (PFDMCH) and their composition and surface properties studied by XPS, grazing-angle Fourier transform infrared spectroscopy and contact angle measurements as a function of time after fabrication as they were stored under ambient conditions for more than 2 years. The spontaneous ambient oxidation of PFDMCH plasma polymers was found to be a multi-step process. The rapid initial oxygen uptake, assigned to reaction between carbon-centred radicals incorporated into the coating during deposition and in-diffusing atmospheric O2, was similar to that of plasma polymers deposited from hydrocarbon-based monomers (alkanes, alkylamines, alcohols), suggesting that the density of radicals incorporated during deposition was similar. Subsequently, however, the extent of oxidation was much lower for PFDMCH coatings. This can be attributed to the lack of availability of hydrogen abstraction reactions, which are important for radical propagation in hydrocarbon-based plasma polymers. While XPS recorded a continuous incorporation of oxygen for more than 2 years, the air/water contact angles decreased only during the first 2 months and on further storage remained stable. There appeared to be only a small extent of surface restructuring as assessed from the small depth variations of compositions. The surface was enriched in CF3 groups at all times. © 1998 John Wiley & Sons, Ltd.
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    Part 2. N-[m-(3-(trifluoromethyl)diazirine-3-yl)phenyl]-4- (-3-thio(-1-D-galactopyrannosyl)-maleimidyl)butyramide (MAD-Gal) on diamond Dedicated to Professor Siegfried Hofmann on the occasion of his 60th birthday. (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 793-799 
    Details
    ISSN: 0142-2421
    Keywords: ToF-SIMS ; XPS ; biomaterials ; carbohydrates ; galactose ; patterning ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and x-ray photoelectron spectroscopy (XPS) are used to characterize a newly synthesized glycosylated photoactivatable reagent designed for surface glycoengineering. The glycoaryldiazirine reagent MAD-Gal (N-[m-(3-(trifluoromethyl)diazirine-3-yl)phenyl]-4-(-3-thio(-1-D- galactopyrannosyl)-maleimidyl)butyramide) is immobilized with 350 nm light on diamond surfaces. The XPS atomic constituents and chemical shifts, as well as ToF-SIMS-specific characteristic fragments of the photoimmobilized molecule, are identified. The grafting on oxygen-containing sites previously observed for N-(m-(3-(trifluoromethyl)diazirine-3-yl)phenyl)-4-maleimido-butyramide (MAD) is confirmed. The difference in grafting efficiency for fresh and aged substrates indicates that other still unidentified reaction sites could be involved. The ToF-SIMS imaging is used to exhibit the ability to pattern the surface with the glycosylated aryldiazirine. © 1998 John Wiley & Sons, Ltd.
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    Interfacial interactions of plasma-polymerized acrylic acid and an oxidized aluminium surface investigated using XPS, FTIR and poly(acrylic acid) as a model compound (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 961-973 
    Details
    ISSN: 0142-2421
    Keywords: interface ; aluminium ; plasma polymer ; acrylic acid ; XPS ; FTIR ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) are used to characterize the interface between poly(acrylic acid) (PAA) and an aluminium oxyhydroxide (AlOOH) surface. Reaction of the PAA carboxylic acid functionality with hydroxyl groups at the surface of the oxide to form a monodentate carboxylate complex —C(=O)—O—Al was identified by FTIR. The degree of conversion of the acid to the salt at the interface was estimated to be 40% from the XPS analysis of PAA overlayers of varying thickness. An equivalent reaction was identified at the interface between AlOOH and a monolayer of strongly bonded plasma-polymerized acrylic acid (ppAAc) that remained after solvent washing. The resistance of the monolayer of ppAAc to solvent washing was attributed to the formation of interfacial carboxylate complexes with the AlOOH surface. © 1998 John Wiley & Sons, Ltd.
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    Substrate Effects and Chemical State Plots for the XPS Analysis of Supported TiO2 Catalysts (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 292-294 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; Auger parameter ; TiO2 ; catalyst ; chemical state plot ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The analysis by XPS of TiO2 deposited on different substrates (SiO2, MgO, Ag, SnO) shows the existence of shifts in the Ti 2p binding energy and Auger parameter values. The magnitude of these shifts is a function of the support and of the coverage. A systematic representation of these shifts is possible with a chemical state plot. The implications of the existence of such shifts for the characterization of catalysts are discussed. © 1997 by John Wiley & Sons, Ltd.
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    X-ray Photoelectron Spectroscopic Studies of Carbon-fiber Surfaces. 21. Comparison of Carbon Fibers Electrochemically Oxidized in Acid using Achromatic and Monochromatic XPS (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 409-417 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; carbon fiber ; achromatic ; monochromatic ; oxidize ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Amoco M40 PAN-based carbon fibers were electrochemically oxidized in a pilot plant system. The changes in the surface of the fibers were monitored using monochromatic x-ray photoelectron spectroscopy (XPS). A parallel experiment using achromatic x-radiation was conducted for comparison. Other graphitic materials were also studied. Decomposition of the fiber due to x-ray exposure could be effectively eliminated by using the monochromator. The use of monochromatic x-radiation produced considerable narrowing in the linewidth of the graphitic peak. This allowed the curve fitting of the component peaks to be performed with significantly greater confidence. © 1997 John Wiley & Sons, Ltd.
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    Elastic Scattering Corrections in AES and XPS. II. Estimating Attenuation Lengths and Conditions Required for their Valid Use in Overlayer/Substrate ExperimentsPaper presented at the 9th International Conference on Quantitative Surface Analysis (QSA-9), Guildford, UK, 15-19 July 1996. (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 430-446 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; AES ; attenuation length ; IMFP ; elastic scattering ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: We examine substrate/overlayer experiments and the equations commonly used to quantify overlayer thicknesses. Comparisons with accurate Monte-Carlo simulations show that using attenuation lengths (rather than inelastic mean free paths) eliminates most of the error due to elastic scattering without increasing the complexity of the quantification.We give attenutation lengths for 27 elements, calculated by the criterion that systematic errors in such quantifications should be minimized. These are therefore the best attenuation length values to use in layerwise quantification. We show that, provided these attenuation length values are used, the error in estimation of the thickness of an overlayer due to elastic scattering can be limited to ±(5%+1 Å) for an emission angle ≤58° from the surface normal, and ±(10%+1 Å) for an emission angle ≤63° from the surface normal. This accuracy is acceptable for most analytical work. Other methods (such as analytical transport theory) are much more complicated, and achieve a high precision that is often unnecessary in view of other uncertainties typically present in these experiments (such as errors due to surface morphology and diffraction effects). The results presented here, using the full theory, show that the analyst's simple straight-line approximation is in fact of adequate accuracy, provided that the correct values of attenuation length are used.Simple semi-empirical equations are presented, which allow the analyst to estimate the attenuation length for electrons of kinetic energy between 50 and 2000 eV, to a standard uncertainty of 6%. © 1997 John Wiley & Sons, Ltd.
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    Evaluation of X-ray-excited Valence Band Measurements for the Determination of the Surface Composition of Model Thermoplastic Olefins (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 643-649 
    Details
    ISSN: 0142-2421
    Keywords: thermoplastic olefin (TPO) ; valence band ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: In this study we evaluate the utility of using x-ray-excited valence band measurements for the determination of the surface composition of simple model thermoplastic olefin systems composed of binary blends of semicrystalline polypropylene (PP) and an amorphous ethylene-propylene copolymer (E-co-P). Blend compositions included combinations of high- and low-molecular-weight (MW) PP and E-co-P composed of 60 wt.% PP/40 wt.% E-co-P and 80 wt.% PP/20 wt.% E-co-P blends. Results demonstrate that experimental valence band spectra for the polyolefin blends can be approximated by a linear combination of the pure-component valence band spectra. Bulk compositions determined from spectra recorded from cryomicrotomed cross-sections were found to be consistent with the bulk component wt.%. The surface compositions of the binary blends were all found to be enriched in PP. Measurements taken from the 60/40 wt.% blends were 10-20% higher in PP concentration than the bulk compositions, and were found to vary depending on the MW combination of the components. No MW dependence was observed for the 80/20 wt.% blends, apparently due to a near saturation of the surface with PP. The development of methods for assessing the surface composition of these types of materials may prove useful in monitoring changes in composition with material formulation and process conditions. Information of this nature could be helpful in permitting an evaluation of potential influences of composition on adhesion. © 1997 by John Wiley & Sons, Ltd
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    Elastic Scattering Corrections in AES and XPS. III. Behaviour of Electron Transport Mean Free Path in Solids for Kinetic Energies in the Range 100 eV〈E〈400 eVPaper presented at the 9th International Conference on Quantitative Surface Analysis (QSA-9), Guildford, UK, 15-19 July 1996. (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 447-453 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; AES ; elastic scattering ; IMFP ; transport mean free path ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Quantitative Auger electron spectroscopy (AES) and x-ray photoelectron spectroscopy (XPS) depend on an accurate knowledge of the correct depth scale of emission of the signal electrons. This depends on both inelastic and elastic scattering processes occurring in the specimen under analysis.A previous paper showed that the depth scale in AES and XPS is significantly influenced by unexpected structure in the transport mean free path for electrons in high-atomic-number elements over the approximate energy range 100-400 eV. This behaviour is implicit in Mott cross-sections, which are known to be reliable and have been used in low-energy electron diffraction (for example) for decades. This paper examines the features of electron-atom elastic scattering over the range of energy and atomic number important in XPS and AES analysis. In particular, the third and fourth partial waves, together with Levinson's theorem are shown to give rise to the structure in the transport mean free path. This is a transport cross-section analogue of the Ramsauer-Townsend effect exhibited at low energies in total elastic scattering cross-sections. © 1997 John Wiley & Sons, Ltd.
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    Surface Analysis of a Hydrothermally Treated H-ZSM-5 Zeolite (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 660-666 
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    ISSN: 0142-2421
    Keywords: XPS ; XAES ; steamed zeolites ; acidity ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The external surface of a hydrothermally treated H-ZSM-5 zeolite was studied with XPS and x-ray Auger electron spectroscopy. It was established that Al removed from tetrahedral framework positions migrated into the outermost layers and produced an Al enrichment. In order to get information on the acidic properties of the outermost layers and of extra-framework Al (EFAl), we investigated the XPS N 1s level of adsorbed ammonia. Two different Brönsted acid sites with N 1s binding energies of 402.3±0.5 and 401.2±0.2 eV, respectively, were found in the untreated H-ZSM-5 zeolite. A third acid site (398.8±0.3 eV) appeared after water vapour treatment, which is probably also a Brönsted acid site. The modified Auger parameter α′ was used for identification of the chemical state of EFAl. The removed Al maintained the tetrahedral coordination, was non-acidic, uncharged, partly soluble in concentrated acetic acid and able to block part of the acid sites. A comparison of acidity between the surface and bulk phase (temperature-programmed desorption results) clearly showed that Al is heterogeneously distributed in the framework. A large part of Al on the surface is not in a framework position and is blocked by EFAl. © 1997 by John Wiley & Sons, Ltd.
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    Quantitative XPS: Influence of Elastic Electron Scattering in Quantification by Peak Shape Analysis (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 404-408 
    Details
    ISSN: 0142-2421
    Keywords: quantitative surface analysis ; elastic scattering ; XPS ; layer thickness ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A new method for non-destructive quantitative analysis of surface nanostructures was developed in recent years. It relies on analysis of the XPS peak shape and usually the effects of elastic electron scattering are neglected in practical applications of the method. In the present paper we study the influence of elastic electron scattering for interpretation of the analysed experimental data. Spectra of the Au 4d peak [with inelastic mean free path (IMFP)=16 Å] from a thin layer of Au atoms situated at varying depths in a Ni solid were analysed. When elastic scattering is neglected, the accuracy of the quantification is ∽10% for depths smaller than 1.5 IMFP but for a depth of 2.5 IMFP the determined quantitative amount of gold is 25% too low. The effect of elastic scattering on the peak intensity was 〈10% for marker depths up to 1 IMFP but it grows to ∽40% at 2.5 IMFP. After correction for elastic scattering effects, the accuracy of the analysis is improved and the root-mean-square scatter in the determined amount of Au around the mean value is reduced from 15.4% when elastic scattering effects are neglected to 11% when they are included in the analysis. For the present system, it is then concluded that the effect of elastic scattering is quite small for marker depths smaller than ∽1 IMFP but for larger depths the effect is substantial. © 1997 John Wiley & Sons, Ltd.
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    Oxidation of molybdenum surfaces by reactive oxygen plasma and O2+ bombardment: an auger and XPS study (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 235-241 
    Details
    ISSN: 0142-2421
    Keywords: molybdenum oxides ; oxygen plasma ; ballistic effects ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The oxidation of molybdenum at room temperature with oxygen plasma or a beam of O2+ ions has been studied with Auger electron spectroscopy (AES) and x-ray photoelectron spectroscopy (XPS). Auger electron spectroscopy shows a progressive modification of the N2,3VV lineshape and the development of new features close to the intense M4,5NN Auger transitions of metallic Mo at 160, 186 and 221 eV. The effects are greater with the oxygen plasma than with the O2+ bombardment. X-ray photoelectron spectroscopy shows that the incorporation of oxygen into the molybdenum gives rise to the formation of Mo6+, Mo4+ and a form of Mon+ (n〈4). The (Mo4++Mon+)/Mo6+ ratio was higher after O2+ ion bombardment than by treatment with the oxygen plasma, in which case the concentration of the Mo4+ and Mo6+ oxidation states was very similar. The analysis of the O 1s and O KLL Auger spectra under the different conditions showed that whenever a high concentration of the Mo6+ species is present, the O-Mo bond is more covalent in character. To evaluate the influence of chemical and ballistic effects in the two oxidation processes, additional experiments were carried out with MoO3. This oxide was bombarded with Ar+ and O2+ until a steady-state surface composition was reached. In both cases, the formation of a considerable amount of Mo4++Mon+ (n〈4) and Mo0 species (i.e. reduction of Mo6+ initially present in the sample) was detected. These results suggest that the high concentration of Mo4++Mon+ found upon bombardment of Mo0 with O2+ is rather produced by ballistic effects, which cause the reduction of the initially formed Mo6+. © 1998 John Wiley & Sons, Ltd.
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    The use of high-resolution XPS and ToF-SIMS to investigate segregation phenomena of minor components of a model coil coating formulation (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 444-454 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; ToF-SIMS ; surface segregation ; coil coatings ; adhesion ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The segregation of minor components - a melamine-formaldehyde resin and a poly(acrylic) flow control agent - in a model epoxy resin coil coating applied to hot-dipped galvanized steel has been investigated by high-resolution XPS and time-of-flight SIMS (ToF-SIMS). It is shown that by using the highest resolution monochromated XPS currently available, the C 1s spectrum can be peak fitted to account for all eleven carbon functionalities present in the three components of the organic coating. A ToF-SIMS analysis of the melamine-formaldehyde resin has been undertaken and a comprehensive ion fragmentation scheme for the positive ion spectrum of this molecule in the range 0-500 Da is proposed. It is shown, by both surface analytical techniques, that when the flow control agent is excluded from the formulation the surface of the paint film is enriched in the melamine-formaldehyde component. On addition of the flow control agent such segregation is only identified by XPS; the ToF-SIMS spectrum resembles that of the flow control agent. This is taken to be an indication of monolayer segregation of this component at the paint/air interface. Such segregation phenomena are shown to be insensitive to substrate surface pretreatment. © 1998 John Wiley & Sons, Ltd.
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    Depth distribution and bonding states of phosphorus implanted in titanium investigated by AES, XPS and SIMS (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 471-479 
    Details
    ISSN: 0142-2421
    Keywords: AES ; SIMS ; XPS ; implantation ; phosphorus ; titanium ; depth profiling ; bonding ; phase formation ; factor analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The depth distribution of phosphorus implanted in titanium at 20 keV with doses ranging from 1×1015 to 3×1017 cm-2 was investigated by AES, SIMS and XPS. For small doses (≤1016 cm-2) Gaussian-like phosphorus profiles have been observed. For doses 〉1017 cm-2 the depth profiles suggest that a TiP-like surface layer is formed without additional thermal treatment. In the implanted layer a certain amount of oxygen was found.Factor analysis of the spectra obtained during AES and XPS depth profiling proved that the surface region of the implanted samples is composed of Ti metal, surface oxide and Ti phosphide, which is produced at high doses.From P L2,3 VV Auger spectra the existence of a second bonding state of phosphorus is deduced, which is distinguished from TiP by differences in the peak shape and position. This species is distributed mainly in a narrow profile located at a depth near the projected range of the phosphorus ions, i.e. in the region of maximum lattice defects. It is attributed to phosphorus on interstitial sites. The amount of this species reaches saturation for a dose of ∽1017 cm-2. © 1998 John Wiley & Sons, Ltd.
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    Surface spectroscopic study of the behaviour of a thin TiN layer as protective coating of iron against corrosion by humid SO2-aggressive environments (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 667-673 
    Details
    ISSN: 0142-2421
    Keywords: TiN coatings ; XPS ; AES ; ICEMS ; SO2 corrosion ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: In this work the behaviour of thin (30 nm), single-layer TiN coatings on iron in different humid SO2-aggressive environments [(i) [SO2]=0.001% v/v, 80% relative humidity; (ii) [SO2]=0.001% v/v, 98% relative humidity; (iii) [SO2]=0.04% v/v, 80% relative humidity; (iv) [SO2]=0.04% v/v, 98% relative humidity] has been studied by integral conversion electron Mössbauer spectroscopy (ICEMS), XPS, AES and scanning auger microscopy (SAM). The results show that in atmosphere (i) there is no degradation of either the TiN coating or the underlying iron even after 14 days of exposure, whilst in atmosphere (iv) the TiN coating is completely destroyed after 7 days of exposure. In other cases the XPS data show that there are no significant chemical changes in the TiN coatings with exposure time; however, the ICEMS data show that after a sufficiently long exposure period, whose duration depends on the characteristics of the SO2 atmosphere, the underlying iron corrodes to give Fe2+ and Fe3+ species. This is attributed to the existence of small pores in the TiN coating, which allow the permeation of SO2, O2 and H2O from the atmosphere to the TiN/Fe interface. © 1998 John Wiley & Sons, Ltd.
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    Investigation of the surface of vanadyl pyrophosphate catalysts (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 736-741 
    Details
    ISSN: 0142-2421
    Keywords: vanadyl pyrophosphate catalysts ; XPS ; ISS ; surface P/V ratio ; Cs+-doped (VO)2P2O7 catalysts ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The surface composition of (VO)2P2O7 catalysts was investigated by x-ray photoelectron spectroscopy (XPS) and ion scattering spectroscopy (ISS). The P/V ratio on the surface of (VO)2P2O7 catalysts from aqueously prepared precursors lies between 1.3 and 1.4, based on XPS calibrations with different VPO glasses as standard materials. With ISS we obtained a higher P/V ratio of (VO)2P2O7 catalysts in the outermost layer of ∽2-3.The addition of caesium (Cs+) caused a further increase in the P/V ratio of the surface of (VO)2P2O7 with increasing Cs+ concentration. Ion scattering spectroscopy indicated that Cs+ was mainly confined to the uppermost layers, and at high doping concentrations a total surface coverage with Cs+ was achieved.The influence of water vapour on the surface composition of the catalysts was also investigated. A migration and a loss of phosphorus was found after and during water vapour treatment using XPS, ISS and thermogravimetric measurements. The surface of (VO)2P2O7 is assumed to be a dynamic system influenced by the partial pressure of water vapour in the gas phase. The rate of bulk oxidation of (VO)2P2O7 was dependent on the water vapour content in the gas phase. © 1998 John Wiley & Sons, Ltd.
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    Interdiffusion at the Al2O3/Ti interface studied in thin-film structures Dedicated to Professor Siegfried Hofmann on the occasion of his 60th birthday. (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 861-867 
    Details
    ISSN: 0142-2421
    Keywords: AES depth profiling ; XPS ; metal/oxide thin-film structures ; Al2O3/Ti interface ; interdiffusion ; interfacial reactions ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The early-stage interfacial reactions between amorphous Al2O3 (a-Al2O3) and crystalline α-Ti (c-Ti) thin films were studied in thin-film structures with two different thicknesses. Smooth silicon (111) substrates were covered firstly with a TiN thin-film diffusion barrier and then with a crystalline Ti layer. Finally, amorphous Al2O3 was sputter deposited onto the crystalline Ti layer. The samples were heated in a differential scanning calorimeter with a linear heating rate of 40°C min-1 - from room temperature up to different final temperatures of 350-700°C in an argon atmosphere to activate reactions at the a-Al2O3/c-Ti interfaces - and then rapidly quenched. The interdiffusion at the a-Al2O3/c-Ti interface was studied using the rate of change of the reaction width obtained from Auger electron spectroscopy (AES) sputter depth profiles. The beginning of the reaction, which involves the diffusion of oxygen (followed by Al) into the c-Ti thin film, was observed at ∽425°C. The activation energy at the a-Al2O3/c-Ti interface was found to be 1.6 eV for the oxygen diffusion from the amorphous Al2O3 into the c-Ti thin film between 425°C and 650°C, and 0.9 eV for the Al diffusion between 500°C and 625°C. The new crystalline reaction product is composed of α2-Ti3Al phase and a solid solution of oxygen in α-Ti. The influence of different sample structures on kinetic quantities is discussed. © 1998 John Wiley & Sons, Ltd.
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    XPS: binding energy calibration of electron spectrometers 5 - re-evaluation of the reference energies (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 642-649 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; binding energy ; calibration ; reference energies ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The binding energies of the calibration peaks for x-ray photoelectron spectroscopy - Cu 2p3/2, Ag 3d5/2 and Au 4f7/2 - have been reassessed based on the traceable data recorded in 1984 using unmonochromated x-rays and an analyser resolution of 0.3 eV. The changes in those energies, for different x-ray sources and analyser resolutions, have been calculated and the results compared with further data. This includes work with monochromatic Al x-rays recorded at high energy resolution, allowing the binding energies to be referred to a new zero value set at the Fermi edge measured for Ag. A consistent set of data is presented for the calibration and assessment of photoelectron spectrometers with energy resolutions in the range 0.2-1.5 eV, when used with unmonochromated Al or Mg x-rays or monochromated Al x-rays. © 1998 John Wiley & Sons, Ltd.
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    XPS and x-ray diffraction characterization of thin Co-Al-N alloy films prepared by reactive sputtering deposition (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 659-666 
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    ISSN: 0142-2421
    Keywords: XPS ; nanogranular materials ; Co-Al-N ; magnetic materials ; thin film ; nano-composite ; x-ray diffraction ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Thin (Co0.8Al0.2)100-xNx (x=0-30 at.%) alloy films prepared by a reactive radio frequency (r.f.) sputtering method were characterized by XPS and x-ray diffraction (XRD). The film with no nitrogen consisted of a CsCl-type CoAl metallic compound, while the nitrogen-containing alloys were composed of very fine AlN and face-centred cubic (fcc) Co phases. The quantitative XPS analysis under an assumption of uniform distribution of all the elements resulted in much lower concentrations of Co and higher concentrations of Al and N in comparison with the bulk composition for the nitrogen-containing alloys. By taking account of the granular structure of the alloy films, i.e. the nanoscale particles of fcc Co embedded in the AlN compound, the results of quantitative XPS analysis were explained successfully. Moreover, the thickness of the AlN layer and the size of the fcc Co particles were also able to be estimated under the nanoscale structure models. The results were in good agreement with observation by transmission electron microscopy, especially when a nanostructure model was adopted where nanoscale Co-N particles are dispersed in AlN matrix in a simple cubic-like arrangement. © 1998 John Wiley & Sons, Ltd.
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    Investigation of the gas sensing properties of Au/MnOx: response to CO exposure and comparison to Pt/SnO2 (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 1035-1049 
    Details
    ISSN: 0142-2421
    Keywords: sensors ; gold ; manganese oxide ; platinum ; tin oxide ; XPS ; ISS ; x-ray photoelectron spectroscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The surface conductivity changes of 2 at.% Au/MnOx, MnOx and 2 at.% Pt/SnO2 have been measured during cyclical exposures to CO and dry air at 130°C. At each stage of the gas exposures, the corresponding surface compositions were determined using x-ray photoelectron spectroscopy (XPS) and ion scattering spectroscopy (ISS). The results have been used to gain insight into the surface processes that are responsible for the observed conductivity behavior. Upon CO exposure, the extent of conductivity increase is different for each specimen and a synergistic interaction between Au and MnOx is demonstrated. Whereas exposure to dry air (or oxygen) causes the conductivity of Pt/SnO2 to decrease, the Au/MnOx and MnOx specimens continue to exhibit positive changes in surface conductivity. This is believed to be due to sufficiently high partial pressures of oxygen that transform the MnOx-based materials from n-type semiconductors to p-type. The surface analysis data implicate the importance of hydroxyl groups and/or adsorbed water to the CO gas sensing mechanism on all three materials, but there is evidence suggesting that their role is different with respect to Au/MnOx and Pt/SnO2. The potential advantages of combining Au/MnOx and Pt/SnO2 into a single gas sensor are also considered. © 1998 John Wiley & Sons, Ltd.
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    X-ray-induced Metal Reduction in Polymer Hosts (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 46-49 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray-induced metal reduction ; metal-containing polymer ; PdCl2 ; polyvinylpyrrolidone ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: We report the rapid modification of the palladium 3d photoelectron spectrum obtained from a mixed PdCl2/PVP (polyvinylpyrrolidone) film on glass. Chemical transformation of up to one-third of the Pd is observed under XPS analysis conditions that are routinely used for swift survey scans. The alterations can be assigned uniquely to the combination of this x-ray-insensitive metal salt and its polymer host. If this finding can be generalized to other inorganics in or on organic matrices, it has severe implications for the alleged non-destructiveness of XPS surface analysis when addressing certain problems in this technologically increasingly important class of material combinations. © 1997 by John Wiley & Sons, Ltd.
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    Emission-depth Dependence of the Signal Photoelectron Energy Spectrum (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 119-131 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; electron escape depth ; IMSP ; elastic scattering ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: An analytical expression for the escape probability of signal photoelectrons as a function of the depth of origin, energy and direction of emission from a solid has been found by solving a kinetic equation. The solution is expressed by a series of partial escape probabilities corresponding to contributions of electrons that have suffered a certain number of inelastic collisions before leaving a target. The universal relationship between the probability for an electron to escape from a certain depth after being scattered inelastically n times (n=0, 1, 2, …) and the pathlength distribution has been derived. The photoelectron spectra from an Si(Au) tracer located at different depths in an Au(Si) matrix has been calculated analytically and by means of the Monte Carlo technique for different XPS configurations. The peak and the background regions have been found to be strongly affected by elastic scattering of electrons in the sample. The neglect of the elastic collisions has been shown to over- or underestimate the photoelectron current (up to 100% in the case of the Au sample and the Si tracer located at a depth of the order of several inelastic mean free paths). The analytical theory predictions are compared with the corresponding Monte Carlo data and good agreement in absolute units is observed. The obtained results indicate that the assumption of a simple exponential attenuation of electrons made in non-destructive depth-profile reconstructions seems to be less valid in the case of materials in which elastic scattering is significant. © 1997 by John Wiley & Sons, Ltd.
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    Ion Beam Modification of InSe Surfaces (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 111-118 
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    ISSN: 0142-2421
    Keywords: ion bombardment ; InSe ; XPS ; layered material ; spectral processing ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Ion beam modification of InSe (single crystals and molecular beam epitaxy-grown thin films on Si(111) substrate) by Ar+ and O+ (3 keV beam energy) is studied by XPS. The Ar+ ion bombardment produces surface layer enrichment in metallic indium with a gradient of concentrations, i.e. the top surface layer (10-15 Å) contains less metallic indium as compared to the modified layers under it. Bombardment with O+ ions produces an indium oxide layer (∽20 Å thick) on top of InSe. The relevance of the observed ion beam modifications to the preparation of solid state microbattery structures is discussed. © 1997 by John Wiley & Sons, Ltd.
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    Differential charging in XPS. Part III. A comparison of charging in thin polymer overlayers on conducting and non-conducting substrates (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 904-912 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; charging ; polymer ; overlayers ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Previous work has used small-area and imaging XPS to show that differential charging in bulk insulators develops as a result of non-uniform x-ray flux across the surface, causing lateral differential charging. Charging in heterogeneous samples can be further affected by the local sample environment and sample mounting. The current work extends these studies through an analysis of differential charging effects in thin overlayers on conducting and insulating substrates. The charging observed in PnBMA overlayers on indium tin oxide, glass, Ag and Al is discussed as a function of substrate conductivity and photoelectron cross-sections. Substrate conductivity is the most significant factor in determining the magnitude of the overlayer charging observed when no charge compensation is utilized. Differential charging in the PnBMA overlayer was used to image a patterned substrate containing insulating and conducting areas. © 1997 John Wiley & Sons, Ltd.
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    Application of XPS and factor analysis for non-conducting materials (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 942-947 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; factor analysis ; charging effects ; depth profiling ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Data analysis with multivariate mathematical methods is commonly used more and more also for applications in electron spectroscopy. This paper concerns the use of factor analysis in x-ray photoelectron spectroscopy and is focused on the problems occurring during investigations of non-conducting materials. Possibilities of the correction of the charging effect are discussed, considering the aspects of background subtraction and spectra concatenation. The efforts of the proposed procedures are demonstrated with model experiments and depth profile measurements. © 1997 John Wiley & Sons, Ltd.
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    XPS Study of the Segregation of Minor Elements at the Surface of a Commercial Copper-10 wt.% Nickel Alloy (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 747-754 
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    ISSN: 0142-2421
    Keywords: XPS ; copper-nickel ; surface segregation ; oxidation ; annealing ; impurity influence ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: X-ray photoelectron spectroscopy has been used to examine the effects of industrial reduction treatments on the composition and structure of the topmost layers of a commercial copper-10 wt.% nickel alloy (Cu-10Ni).The surface analytical studies carried out on the as-received alloy show, in addition to the usual surface contamination, the formation of nickel(II) hydrated species and pronounced segregations of additive alloying components. Strong enrichments of minor elements are also observed in the outermost layers of the material. Moreover, metallic copper and nickel-based compounds are homogeneously distributed within the segregants in the surface film. Comparison of the surface composition of samples treated in various controlled-reducing atmospheres with a mechanically cleaned alloy surface gives access to the mechanisms responsible for the segregations.The diffusion of the various chemical species is discussed in terms of oxygen potential, leading to concentration gradients of metallic elements. © 1997 by John Wiley & Sons, Ltd.
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    Energy Calibration of X-ray Photoelectron Spectrometers. II. Issues in Peak Location and Comparison of Methods (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 777-787 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; energy calibration ; peak location ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: An analysis is presented of issues involved in peak location for the calibration of the binding energy (BE) scales of x-ray photoelectron spectrometers. These issues include the effects of peak asymmetry, the surface core-level shift, and the avoidance of a sloping background when fitting spectra for energy calibration purposes. Examples of uncertainty budgets for BE measurements are then presented in which illustrative values are shown for the repeatability standard deviation (for repeated BE measurements of the same calibration peak), the expanded uncertainty (at the 95% confidence level) for BE measurements following calibrations based on different numbers of peak measurements, and the tolerance for BE-scale drift and non-linearity for two chosen values (±0.1 and ±0.2 eV) of the total expanded uncertainty for a BE measurement (at the 95% confidence level). It is recommended that a user prepare an uncertainty budget of this type to show clearly the sources of random and systematic error in BE measurements following a calibration.The reference data published by the UK National Physical Laboratory for BE-scale calibration were obtained from fits with a quadratic function to a group of points comprising the top 5% of each peak. Most commercial x-ray photoelectron spectrometers have software available for spectrum synthesis, and we consider here the use of the commonly available Lorentzian, Gaussian, and asymmetric Gaussian functions for peak location. Illustrative fits with Cu 2p3/2 spectra (measured with unmonochromated Al x-rays) showed that comparable accuracy and precision could be obtained with Lorentzian and Gaussian functions as with the quadratic-equation method when different fractions of the peak were fitted. For this asymmetrical line, the asymmetric Gaussian function allowed better accuracy and precision to be obtained with a greater fraction of the line than was possible with the symmetrical functions. © 1997 by John Wiley & Sons, Ltd.
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    Correction for the effects of adventitious carbon overlayers in quantitative XPS analysis (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 924-930 
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    ISSN: 0142-2421
    Keywords: Adventitious ; analysis ; carbon ; contamination ; XPS ; quantification ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A data processing procedure is described that enables the energy-dependent attenuation of the substrate XPS signals from typical samples exhibiting adventitious carbon contamination to be objectively and quantitatively compensated when obtaining elemental analyses from the XPS peak intensities. The procedure is based on well-established theory for a uniform overlayer on a homogeneous substrate, and is evaluated using two representative substrates: oxidized sheet zinc and pressed pellets of sodium fluoride. Suitable values for key parameters are recommended, and an application program in MS-DOS Q-BASIC is available via the Internet. © 1997 John Wiley & Sons, Ltd.
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    Overlayer corrections in XPS (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 352-358 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; peak attenuation ; overlayer effects ; quantitative surface analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: It appears that the same scaling law applies to the attenuation of bulk XPS signals by thin uniform overlayers on rough surfaces, on powdered samples or when using an electron spectrometer with a magnetic immersion lens (i.e. one that integrates the intensity over all ejection angles). A simple but accurate analytical approximation of the attenuation function for these cases will be provided. The existence of a ‘magic’ detection angle of ∽40-45°, where the possible effects of roughness, etc. can be ignored, follows logically from this analysis. First, however, it is argued that while thickness estimates of overlayers are generally rather unreliable due to a lack of knowledge of the necessary material parameters, the corrections applied to the bulk concentrations are usually fairly precise. © 1998 John Wiley & Sons, Ltd.
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    Determination of the concentration of surface hydroxyl groups on metal oxide films by a quantitative XPS method (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 549-564 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; angle-resolved ; Al ; hydroxyl ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Quantitative XPS has been used to determine the surface concentration of hydroxyl groups in native air-formed oxide films on metals having low surface areas. A mathematical expression has been derived to give the concentration of surface hydroxyl groups as a function of the intensity ratio of the OH to O2- contributions to the O 1s photopeak. This expression is based on modeling the oxide film on a metal to be a multilayer system consisting of an outermost layer of organic contamination, a layer of chemisorbed water, a surface hydroxylated region of the oxide film and the inner portion of the oxide film. The average values of the experimentally determined concentrations of surface hydroxyl groups are 15, 13, 11, 6 and 8 OH nm-2 for oxide-covered aluminum, chromium, titanium, tantalum and silicon, respectively. X-ray photoelectron spectroscopy depth profiles using argon ion sputtering and variable-angle XPS have been utilized in this work. Surface treatments have employed either ultrasonic cleaning with organic solvents or argon plasma treatment. © 1998 John Wiley & Sons, Ltd.
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    Energy calibration of X-ray photoelectron spectrometers. Part III: Location of the zero point on the binding-energy scale (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 606-614 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; calibration ; Fermi energy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Calibration of the binding energy scale in x-ray photoelectron spectroscopy (XPS) requires location of the zero point. This zero point has previously been identified with the inflection point in the Fermi-edge region of a valence-band photoemission spectrum of nickel. Comparison of photoemission spectra of nickel and silver measured with monochromated x-rays shows that the inflection points near the Fermi edge differ by 45±5 meV (where the stated uncertainty indicates the standard uncertainty) at an instrumental energy resolution of 0.30 eV. This difference is due to differences in the valence-band densities of states (DOS) of the two metals. Simulations of the Ni photoemission spectrum have been performed based on the DOS calculated by Eckhardt and Fritsche, and the simulated spectrum agrees well with the measured spectrum in the near-edge region. Additional simulations of the Ni photoemission spectrum have been carried out with both monochromated Al x-rays and unmonochromated Mg and Al characteristic x-rays to determine how the Ni near-edge inflection point varies with the energy resolution of the electron energy analyzer in XPS. © 1998 John Wiley & Sons, Ltd.
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    Surface Spectroscopic Studies of Factors Influencing Xanthate Adsorption on Coal Pyrite Surfaces (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 64-70 
    Details
    ISSN: 0142-2421
    Keywords: coal ; pyrite ; xanthate ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The relative adsorption of fluoroxanthates on several different coal pyrites has been found to depend on the degree to which the pyrite surfaces are oxidized. Maximum xanthate adsorption occurs in the absence of pyrite surface oxidation and is affected by the presence of polysulfides and metal-deficient sulfides on the pyrite surface. The structure and electronic properties of the xanthate molecule may also affect its adsorption. 3-(Trifluoromethyl)benzyl xanthate was found to selectively adsorb on pyrite vs. coal surfaces. Secondary ion mass spectrometry is a viable alternative to x-ray photoelectron spectroscopy for detecting xanthate adsorption. © 1997 by John Wiley & Sons, Ltd.
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    Using XPS to Investigate Fiber/Matrix Chemical Interactions in Carbon-fiber-reinforced Composites (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 53-63 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; carbon fibers ; composites ; polyimide ; vinyl ester ; polyphenylene sulfide ; epoxy ; adhesion ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: With the uses of composites expanding into areas from aerospace to recreation, different matrices are being investigated to tailor the composites to specific uses. The degree of adhesion between the fiber and matrix has been recognized to be a critical factor in determining the performance of fiber-reinforced composites. Indirect analysis of the matrix/fiber interface is possible using model compounds which represent functional groups present in the matrix system. Model compounds based on epoxy, polyimide, polyphenylene sulfide and vinyl ester matrices have been investigated to characterize the chemical reactions at the fiber/matrix interface. X-ray photoelectron spectroscopy has been used to characterize both the carbon-fiber surfaces and the reacted carbon-fiber surfaces. The model compounds for the polyimide and polyphenylene sulfide matrices have been found to show little chemical interaction with the fiber surfaces, while chemical reactions have been observed in the vinyl ester and epoxy resin model compound/fiber interfaces. © 1997 by John Wiley & Sons, Ltd.
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    Quantitative Analysis of Palladium Oxide by Means of the Palladium M4,5N1N2,3 Transition (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 132-134 
    Details
    ISSN: 0142-2421
    Keywords: palladium ; particles ; AES ; XPS ; oxidation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The palladium M4,5N1N2,3 transition, which is almost absent in palladium metal, becomes quite intense in palladium oxide. The intensity of the transition is linearly proportional to the amount of palladium oxide. This means that AES can be used for quantitative analysis of palladium oxide layers or supported palladium oxide particles.© 1997 by John Wiley & Sons, Ltd.
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    Simulation of Energy Distribution for Scanning X-ray Probe (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 202-208 
    Details
    ISSN: 0142-2421
    Keywords: diffraction ; elliptical mirror ; energy distribution ; Fermi edge ; monochromator ; optical ray tracing ; rocking curve ; scanning x-ray probe ; simulation ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The energy distribution of a scanning x-ray probe which is equipped with an elliptical mirror monochromator has been simulated with optical ray tracing, a numerically described energy distribution of Al Kα x-ray and a rocking curve. The rocking curve was estimated by dynamic diffraction theory with structure factors for quartz. The peak energy of the diffracted x-ray beam did not change with beam size, although the shapes of energy distribution were found to change slightly. Using the simulated x-ray energy distribution and the apparatus function, the energy width of the Fermi edge was simulated, which is to be compared with that obtained experimentally by monochromatic Al Kα x-ray excitation. The widths of the silver Fermi edge spectra were measured with different x-ray beam sizes. In addition, the relation between the x-ray beam position on the anode and the diffracted x-ray energy distribution was investigated. The peak energy of the diffracted x-ray beam was found to move with the x-ray beam position. It is shown that this kind of simulation can be effectively used for estimating the energy distribution and the intensity distribution of the diffracted x-ray beam. © 1997 by John Wiley & Sons, Ltd.
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    Universality Classes of Inelastic Electron Scattering Cross-sections (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 137-154 
    Details
    ISSN: 0142-2421
    Keywords: inelastic electron scattering cross-section ; XPS ; AES ; REELS ; quantitative surface analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Quantitative XPS and AES analysis of surfaces requires models to do fast calculations of the energy loss of electrons at any energy as they move in solids of general and non-uniform composition. This is possible with the Universal cross-section that was introduced a decade ago. A critical review is given of the Universal cross-section in the light of the results of research carried out since then. In particular its validity is compared to that of experimental cross-sections determined by analysis of reflected electron energy-loss spectroscopy (REELS) spectra. It is shown that for applications in quantitative surface analysis by XPS and AES, the solids can be divided into classes according to the full width at half-maximum of the dominating shape of the inelastic scattering cross-section. The Universal cross-section is quite accurate for solids with a cross-section width 20 eV. For solids with a cross-section width of 10-15 eV, the Universal cross-section is still fairly good for the description of the far-peak region (30 eV from the peak energy) but it is less accurate to account for the near-peak region (10 eV from the peak energy). For solids with a cross-section width 5 eV, the REELS cross-section is always more accurate than the Universal cross-section. A Three-parameter Universal cross-section was defined, which gives a good fit to narrow experimental cross-sections. Parameters for different solids were determied and it was shown that the polymers form a separate universality class. © 1997 by John Wiley & Sons, Ltd.
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    Trajectory Weighting: a Fast Monte Carlo Method for Calculating Large Numbers of XPS/AES Spectra (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 275-284 
    Details
    ISSN: 0142-2421
    Keywords: Efficient Monte Carlo simulation ; XPS ; AES ; quantitative spectrum analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A new, efficient, hybrid Monte Carlo method (‘trajectory-weighting’ method) for the calculation of XPS and AES spectra is presented. The method produces, in one single calculation, XPS or AES spectra for a large number of sample compositions. The method consists of a conventional Monte Carlo calculation for a single standard composition plus transformations for many other compositions. The transformations are based upon proper weighting of the electron trajectories constructed for the standard composition. The weighting factors depend on the elastic and inelastic scattering cross-sections. The trajectory-weighting method has been tested against a conventional Monte Carlo simulation and an analytical model. Furthermore, it has been applied to establish the XPS spectrum dependence on thickness, depth and composition of a buried layer in an otherwise homogeneous sample. © 1997 by John Wiley & Sons, Ltd.
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    An XPS and AFM study of polypyrrole coating on mild steel (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 837-854 
    Details
    ISSN: 0142-2421
    Keywords: polypyrrole ; toluene sulphonate ; steel ; AFM ; XPS ; morphology ; interface ; corrosion ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: We have characterized electrically conductive polymer, polypyrrole (Ppy), films on mild steel with atomic force microscopy (AFM) and x-ray photoelectron spectroscopy (XPS). The Ppy films were polymerized electrochemically from sodium p-toluene sulphonate (ToS) water-ethanol solution. A very good corrosion protective effect of those films on mild steel has been observed previously. After drying in air, thin Ppy films (∽200 nm) were highly adhesive, whereas thicker films (∽7.5 μm) could easily be peeled off from the metal. All films had a nodular surface structure. Thin films were very smooth and their roughness increased with their thickness. The AFM study of the interface between the metal and the polymer showed areas of different morphology, which suggests that adhesive and cohesive failure of the polymer film occurs. A strong variation of the chemical composition at the interfacial layer was observed. A sulphur-rich layer was formed at the interface, indicating that the counter-anions (ToS) were accumulated on the surface of the metal. High-binding energy iron and imine-type nitrogen were detected in a thin Ppy film. Moreover, thin films were substantially overoxidized. The number of anions incorporated into the Ppy matrix varied as a function of film thickness: the ‘doping level’ was about 30% for thicker films and only 12% for thin ones. Nitrate counter-anion-containing Ppy films were also studied in some cases for comparison. © 1997 John Wiley & Sons, Ltd.
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    XPS, XANES and ToF-SIMS Characterization of Reactively Magnetron-sputtered Carbon Nitride FilmsPresented at ECASIA'95 Montreux, Switzerland, October 1995 (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 827-835 
    Details
    ISSN: 0142-2421
    Keywords: carbon nitride ; PVD ; hybridization ; AES ; XPS ; XANES ; ToF-SIMS ; magnetron-sputtered film ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The existence of β-C3N4 with hardness characteristics similar or better than diamond was predicted in 1990 by Liu and Cohen. Many studies have since been devoted to the synthesis of this compound. In the present work, carbon nitride films were deposited by various reactive magnetron sputtering processes of graphite targets in pure nitrogen and characterized by AES, XPS, x-ray absorption near-edge structure (XANES) and static time-of-flight SIMS (ToF-SIMS). Various bonding states (single and double bond) are observed between carbon and nitrogen atoms and between carbon atoms but there is no evidence in the XANES results for either the presence of carbon-nitrogen triple bonds or a pyridine-like ring structure. Surface N/C ratios were estimated to be close to 0.3. Carbon K-edge XANES lineshapes, the C 1s plasmon-loss structure and the calculated density (2.2 g cm-3) indicate that the films are similar to diamond-like carbon without long-range ordering. The presence of CxNy fragments with 1≤y〈4 and the low abundance of CHx and CHxNy fragments in ToF-SIMS spectra further confirm that the carbon atoms do not adopt a graphite or pyridine-like cyclic two-dimensional structure and that the films are not significantly hydrogenated. A three-phase solid solution model is proposed for the composition of the films: a ‘free’ carbon phase, an sp3 - carbon-nitrided phase and an sp2 - carbon-nitrided phase. The relative proportion of these phases is influenced by the deposition conditions. Enhanced plasma ionization reactive magnetron sputtering leads to higher density and to a higher fraction of the sp3 carbon phase. © 1997 by John Wiley & Sons, Ltd.
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    Model for Analysis of XPS Electron Take-off Angle Experiments in Layer-structured Samples: Determination of Attenuation Lengths in a Well-characterized Langmuir-Blodgett Film (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 650-659 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; electron take-off angle ; layered structure ; attenuation length ; Langmuir-Blodgett film ; AFM ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A series of equations have been proposed to calculate take-off angle dependency of the elemental composition of layer-structured models from the experimentally obtained peak intensities of XPS. We have measured the take-off angle dependency of XPS peaks of O 1s, C 1s, Si 2p and Cd 3d from a well-characterized one-layer Langmuir-Blodgett (LB) film of polymerized cadmium 10,12-pentacosadiynoate on a silicon wafer substrate and have applied the newly proposed equations to deduce attenuation lengths of photoelectrons for every element in the layer-structured organic materials. From the best fitting between the theoretically calculated and the experimentally obtained data by the least-squares method, attenuation lengths for a monolayer film of polymerized cadmium 10,12-pentacosadiynoate have been evaluated to be 3.4, 3.7, 4.0 and 4.5 nm for the respective photoelectrons of O 1s (955 eV), Cd 3d5/2 (1082 eV), C 1s (1202 eV) and Si 2p (1388 eV) with the kinetic energy dependency of E0.75. It is essential to use polymerized LB films and to confirm the surface structure of the film directly by suitable techniques such as atomic force microscopy, scanning electron microscopy or transmission electron microscopy.© 1997 by John Wiley & Sons, Ltd.
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    TPD, XPS and ESR Studies of the Surface Processes Involved in the Oxidation of n-Pentane on a (VO)2P2O7 System (1997)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 25 (1997), S. 667-676 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; ESR ; temperature-programmed desorption ; vanadium phosphate ; selective oxidation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Surface-sensitive techniques such as XPS, temperature-programmed desorption-mass spectrometry (TPD-MS) and electron spin resonance (ESR) have been used to study the effect of O2 treatment on the interaction of n-pentane with the surface of an ‘equilibrated’ (VO)2P2O7 catalyst. The study was carried out by means of TPD studies after the catalyst had been in contact with n-pentane at 613 K in the presence and in the absence of O2 and by comparing the results, depending on whether the sample was subjected or not to O2 pretreatment at 613 K previously, to n-pentane adsorption. The valence state of vanadium and the changes in the short-range order around vanadium at the surface after former pretreatments were studied by XPS and ESR techniques, respectively. It was concluded that no oxygen radicals can be created on this catalyst, thus excluding the possibility that these kinds of radicals are involved in the oxidation process. On the other hand, despite the fact that the valence state of vanadium at the surface is an important variable, surface topology around vanadium centres at the surface of the ‘equilibrated’ (VO)2P2O7 sample clearly influences the interaction of n-pentane with the surface. The short-range order around the vanadium sites does not seem to have much effect on the first steps of interaction of n-pentane on the catalyst, but instead alters the further oxidation processes acting on the molecules resulting from the first steps.© 1997 by John Wiley & Sons, Ltd.
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    Surface characterization of PVP-sized and oxygen plasma-treated carbon fibers (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 39-55 
    Details
    ISSN: 0142-2421
    Keywords: carbon fiber ; plasma surface treatment ; sizing ; atomic force microscopy ; x-ray photoelectron spectroscopy ; XPS ; AFM ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The objectives of this work were to characterize the surface of commercial carbon fibers, focusing on the effect of polymer sizing and the effect of oxygen radiofrequency plasma treatment. The fiber surface composition was determined by x-ray photoelectron spectroscopy (XPS) and the surface topography was examined by scanning transmission electron microscopy (STEM) and atomic force microscopy (AFM).Voltage-contrast XPS distinguished between unsized and sized carbon fibers, by which the former behaved as a conductive material whereas the latter behaved as a mixture of both conductive and non-conductive materials due to a contribution from a polymeric sizing material. The AFM measurements revealed that oxygen plasma treatment for 30 s roughened the unsized fiber surfaces; however, further treatment smoothed the overall topography. Oxygen plasma treatment for 30 s also increased the surface oxygen content. © 1998 John Wiley & Sons, Ltd.
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    Some aspects of the fitting of XPS core spectra of polymers (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 204-212 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; polymers ; least-squares fitting ; inelastic background ; Voigt function ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Determination of chemical structure by means of XPS through least-squares fitting of core lines is a widely used method. We present a model for the description of XPS core lines from polymers under simultaneous consideration of the lineshape and the inelastic background. For proper consideration of the background, a model loss function with free parameters was included in the fitting process. The free parameters of the model can be found by least-squares fitting. Using this procedure, XPS core lines of many polymers can be described over a range of 25 eV, which will be demonstrated for selected polymers (PcI, PGMA, PVMK, PPG, PVME, PAA, PE). The model could be easily modified to fit other classes of materials. It will be shown how statistical analysis of the data can be used to evaluate the fitting results. © 1998 John Wiley & Sons, Ltd.
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    High-resolution X-ray photoelectron spectroscopy on giant magnetoresistive CoAg granular films sandwiched between Pt layers (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 30-38 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; AES ; CoAg granular film ; CoPt alloy ; magnetoresistance ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The chemical state of Co, Ag and Pt in giant magnetoresistive CoAg granular films sandwiched between Pt layers is studied using high-resolution x-ray photoelectron spectroscopy. Measurements were carried out as a function of depth for samples deposited at different temperatures and containing different amounts of Co. In all samples Ag is found to segregate at the surface to form an AgPt alloy. The depth profiles are consistent with the deposited Co concentration modified by preferential sputtering. No variation of the chemical state for Co or Ag in the CoAg layer is found for different deposition conditions. However, small amounts of Pt do affect the Co 3d electrons. © 1998 John Wiley & Sons, Ltd.
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    Effect of magnesium ions on the protective power of corrosion products formed on the surface of Al 6061 T6 alloy-10% Al2O3 (v/v) composite in solutions containing chlorides (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 524-530 
    Details
    ISSN: 0142-2421
    Keywords: corrosion ; aluminium matrix composite ; chloride solutions ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: An XPS study of corrosion products formed in seawater and in NaCl solutions on the surface of Al 6061 T6 alloy-10% Al2O3 (v/v) composite was carried out in order to investigate the influence of chloride and magnesium ions (coming from corrosive solutions) and inhomogeneity of the metallic matrix due to the presence of inter-metallic compounds segregated at the grain boundaries.Potentiodynamic polarization tests were carried out to evaluate Al composite resistance to both general and localized attack.Large- and small-area XPS analyses were performed to obtain qualitative and quantitative characterization of corrosion layers. The distribution of the most interesting components of corrosion layers was observed with the Auger technique.The results of electrochemical tests, indicating that specimens immersed in NaCl solutions have a lower pitting corrosion resistance, were correlated with the composition of the corrosion layers, showing higher content in Cl compounds where localized corrosion takes place and higher resistance to corrosion where magnesium compounds are co-precipitated with aluminium corrosion compounds. © 1998 John Wiley & Sons, Ltd.
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    XPS: binding energy calibration of electron spectrometers 4 - assessment of effects for different x-ray sources, analyser resolutions, angles of emission and overall uncertainties (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 617-641 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; binding energy ; calibration ; reference energies ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A detailed analysis is made of the binding energy calibration of X-ray photoelectron spectrometers when using monochromated Al Kα x-rays or unmonochromated Al or Mg Kα x-rays. The binding energies of the peaks for Cu 2p3/2, Ag 3d5/2 and Au 4f7/2, as well as for the Ni Fermi edge, are measured at high resolution using monochromated Al Kα x-rays. The apparent binding energy shifts of the peaks are then calculated for this source, and also for the Al and Mg unmonochromated x-ray sources, using full synthetic Kα x-ray structures, as a function of Gaussian spectrometer energy resolutions in the range 0.2-1.5 eV. For all three x-ray sources, the relative binding energies for the Cu 2p3/2 and Au 4f7/2 peaks are contained within ±0.015 eV but the effects for Ag 3d5/2 are stronger and the containment range must be increased to ±0.026 eV. Further data and calculations are provided for surface core-level shifts and here it is found necessary to restrict emission angles to 56° for all the peak separations to be restricted to the above range of ±0.026 eV. Other instrumental effects may give rise to additional larger or smaller effects. Non-optimized settings for monochromators can show further shifts of up to ±0.2 eV.The uncertainties associated with the above calibration are then analyzed to show how the uncertainty at 95% confidence varies across the binding energy range. Example calculations show that seven repeats of both the Cu 2p3/2 and Au 4f7/2 binding energies may be used to define the peak repeatability and that one or two measurements can then be made for each calibration peak to define the calibration. The precise number of measurements to be used depends on the peak energy repeatability and the required confidence limits for the calibration. In practical situations, however, it is likely that the greatest uncertainty in the binding energy scale arises from the drift in the electronics between calibrations. © 1998 John Wiley & Sons, Ltd.
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    XPS studies of the modification of polystyrene and polyethyleneterephthalate surfaces by oxygen and nitrogen plasmas (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 674-681 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; plasma ; contact angle ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Polystyrene and polyethyleneterephthalate surfaces were exposed to helium, oxygen/helium and nitrogen/hydrogen plasmas singly and in combination. The treated surfaces were evaluated by water contact-angle measurements and by x-ray photoelectron spectroscopy. It was found that the oxygen and nitrogen tend to graft to common carbon atoms, to form amide groups. The water wettability was found to correlate with the fraction of electronegative atoms incorporated into the surface. © 1998 John Wiley & Sons, Ltd.
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    Use of aminosilane coupling agent in the synthesis of conducting, hybrid polypyrrole-silica gel particles (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 689-698 
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    ISSN: 0142-2421
    Keywords: polypyrrole ; silica gel ; silane coupling agent ; hybrid materials ; XPS ; thermogravimetry ; electrical conductivity ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A new route for the synthesis of conducting polypyrrole-silica composites is described. Silica gel particles were modified by aminopropyltriethoxysilane (APS) and acted as porous inorganic substrates for the in situ synthesis of polypyrrole (PPy). The resulting polypyrrole-silica-APS hybrid materials were characterized by XPS, thermogravimetric analysis, BET and conductivity measurements. It is found that APS yields a substantial increase in the PPy mass loading (from 6 to 11.5 wt.%) but, more importantly, the hybrid particles obtained are conductive and have a negligible static charge in XPS due to their PPy-rich surfaces. In the absence of any APS treatment, polypyrrole is mainly loaded in the pores of the silica gel so these polypyrrole-silica particles are poorly conductive and charge up during XPS analysis. The conductivity threshold (10-2 S cm-1) was obtained for an APS initial concentration of 1% (v/v). In addition, these conducting hybrid particles have a fairly high specific surface area in the 160-180 m2 g-1 range. © 1998 John Wiley & Sons, Ltd.
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    Simple model for the XPS analysis of polysaccharide-coated surfaces (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 742-747 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; surface modification ; polysaccharides ; cell-resistant surfaces ; polyethyleneimine ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A simple model was developed for the interpretation of results stemming from the XPS analysis of polymer surfaces modified by polyethyleneimine adsorption followed by surface coupling of polysaccharides. Theoretical surface compositions were evaluated from the calculated XPS intensity arising from a layered structure composed of a surface oxidized polymer, an intermediate polyethyleneimine layer and a top polysaccharide layer.Results of calculations were compared to analytical data obtained from fixed-angle XPS analysis of polysaccharide-coated surfaces and to the performances of the latter in in vitro cell adhesion experiments. It is shown that the model can correctly predict the relationship between the experimental surface composition and the cell-resistant properties of polysaccharide-coated surfaces. © 1998 John Wiley & Sons, Ltd.
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    Study of the interfacial chemistry of chlorinated rubber paint on different substrates after the curing process (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 433-443 
    Details
    ISSN: 0142-2421
    Keywords: chlorinated rubber ; metallic substrates ; polymeric sheet substrate ; interfacial degradation ; curing process ; adhesion ; XPS ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The interfacial chemistry of a highly pigmented chlorinated rubber paint applied over aluminium, cold-rolled and stainless steel, copper and zinc metallic substrates and poly(vinyl chloride) (PVC) polymer sheet have been studied using x-ray photoelectron spectroscopy (XPS). The results obtained by XPS were compared with those of bond strength measurements. The XPS analyses reveal significant differences in the failure mode. The chlorinated rubber paint on the PVC polymer sheet displays the highest bond strength value and on the zinc the lowest. Chemical changes, suggesting dehydrochlorination of chlorinated rubber paint in the paint/metal interfacial region, were only observed on the metallic substrates. With the aluminium, stainless steel, copper and zinc substrates, the curing of the chlorinated rubber paint causes the formation of a highly hydrocarbon-enriched interfacial paint surface. In contrast, the chlorinated rubber paint/PVC polymer sheet system shows no change in the interfacial surface composition. © 1998 John Wiley & Sons, Ltd.
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    Quantitative analysis of surface ethylene concentrations in ethylene-propylene polymers using XPS valence bands (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 425-432 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; valence band ; quantitative analysis ; polymer ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Polyolefin surfaces and interfaces can have a substantial effect on polyolefin processing and properties. Despite the importance of these surfaces and interfaces, there have been few good ways of determining the type of polyolefin on a surface. In this work, a quantitative XPS method for the determination of surface ethylene concentrations in ethylene-propylene polymers is presented. Calibration lines are created using differences in the valence band spectra of various polyethylene (PE), polypropylene (PP) and ethylene-propylene polymer (EP) standards. These lines are then used to determine surface ethylene concentrations on propylene-ethylene polymers. This procedure yields accurate ethylene determinations (±5 wt.% ethylene) when surface contamination (such as additives) is low. At higher surface contamination levels, the accuracy of the method degrades unless valence band contributions from the contamination (or additives) are accounted for. When surface additive levels are high, valence band analyses are shown to be useful in determining the nature of the additives present. Valence band spectra obtained from other polyolefins (polyisobutylene, poly-1-butene, poly-1-hexene and poly-1-octene) are also presented. The spectra for polyisobutylene and poly-1-butene are distinctly different from that obtained from PE (also PP). The spectra obtained from poly-1-hexene and poly-1-octene are similar to that obtained from PE, but are distinctly different from those obtained from polyisobutylene, poly-1-butene and PP. This valence band approach for determining surface compositions should be applicable to other mixed polyolefins that have significantly different valence bands. Case studies involving haze on injection-molded plaques and PE cling-films are presented. © 1998 John Wiley & Sons, Ltd.
    Additional Material: 8 Ill.
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    Atomic force microscopy investigation of the O2+-induced surface topography of InP (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 930-938 
    Details
    ISSN: 0142-2421
    Keywords: AFM ; XPS ; surface topography ; InP ; ion bombardment ; x-ray photoelectron spectroscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The surface topography development of InP as a function of O2+ ion energy and incident angle was investigated using atomic force microscopy (AFM). Cone formation was found to be the dominant surface feature under various O2+ ion bombarding conditions. However, variations in the density and size of the cones at different O2+ ion bombardment conditions were observed. The variation of surface topography with O2+ ion bombardment conditions is correlated with changes in InP surface composition. The results support an intrinsic model of cone formation, which postulates that the sputtering of InP causes In enrichment at the surface due to the preferential sputtering of phosphorus from InP. Furthermore, radiation-enhanced surface diffusion results in agglomeration of indium atoms into indium clusters. These indium clusters seed the development of sputter cones due to the difference in sputter rates of InP and indium. © 1998 John Wiley & Sons, Ltd.
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    Electronic Resource
    Standard test data for estimating peak-parameter errors in x-ray photoelectron spectroscopy. I. Peak binding energies (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 939-956 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; reference data ; x-ray photoelectron spectroscopy ; peak fitting ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Standard test data (STD) are simulations of analytical instrument responses that help to determine the veracity of computer-based, data analysis procedures that are typically used with instruments. The STD were developed for determining errors in peak parameters obtained from data analysis algorithms used in x-ray photoelectron spectroscopy (XPS). The STD were mainly C 1s doublet spectra constructed from spline polynomial models of measured C 1s polymer spectra. Different spectra were created based on a replicated factorial design with three factors: peak separation; relative intensity of the component peaks; and fractional Poisson noise. These doublet spectra simulated XPS measurements made on different two-component specimens. Single-peak C 1s spectra for individual polymers were also simulated, to provide the null case for identification of the doublet spectra. Twenty analysts used a variety of data analysis programs and a variety of curve-fitting approaches to determine peak binding energies. Results indicate that data analysis of doublet spectra may be problematic, because up to 50% of the STD doublets were assigned incorrectly as singlets. For spectra that were correctly identified as doublets, bias and random error in peak binding energies depended on the amount of separation between the component peaks and on their relative intensities. Biases ranged from -0.055 eV to 0.34 eV, while random errors ranged from 0.012 eV to 0.13 eV. Use of the Gaussian-Lorentzian function fitted to spectra resulted in smaller biases than the use of a Gaussian function alone. As a guide to evaluating peak energy uncertainties in their own analyses, analysts may find it useful to analyze the STD themselves and then compare their results with those reported here. The spectra may be obtained at http://www.acg.nist.gov/std/main.html. © 1998 John Wiley & Sons, Ltd.
    Additional Material: 16 Ill.
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    XPS studies of low-temperature plasma-produced graded oxide-silicate-silica layers on titanium (1998)
    Chichester [u.a.] : Wiley-Blackwell
    Surface and Interface Analysis 26 (1998), S. 1027-1034 
    Details
    ISSN: 0142-2421
    Keywords: XPS ; x-ray photoelectron spectroscopy ; Ti ; SiO2 ; Auger parameter ; depth profiling ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A method has been developed to produce a silica coating bonded to an oxidized titanium substrate, graded in composition and structure through the surface layer, providing the base for deposition of bioactive glasses and hydroxyapatite. A low-temperature air/water/tetraethoxysilane plasma coating method is reported. Characterization of the graded surface layer using XPS and SEM is compared with previously reported studies of similar layers on nickel substrates. Depth profiling and the modified Auger parameter were used to elucidate the structure of the interphase region between the titanium and silica. A functionally-graded layer, from the titanium metal through the oxide, orthosilicates, pyrosilicates, chain silicates and layer silicates to bulk silica, was demonstrated. The thickness of the layer was in the range 30-50 nm, depending on the duration of oxidation and tetraethoxysilane deposition. © 1998 John Wiley & Sons, Ltd.
    Additional Material: 12 Ill.
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