Quantitative surface microanalysis of samples with extreme topography utilising image interpretation by scatter diagrams and principal component analysis

Barkshire, I. R.; Kenny, Peter G.; Fletcher, Ian; Prutton, M.

doi:10.1016/0304-3991(96)00039-3

Cited by 14 publications

(9 citation statements)

References 18 publications

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“…Images were collected over a range covering the Ni 2p 3/2 envelope of 848 eV-870 eV at an interval of 0.2 eV, using medium magnification (400 ð 400 µm), an 80 eV pass energy, imaging aperture 2, charge neutralizer set to 1.6 A, 2.8 eV, and a dwell time of 240 s. X-ray focusing was assisted by drilling two holes into the surface of the Ni metal to produce regions of zero photoelectron counts. Our procedure is similar to that used by Barkshire et al,18,19 Prutton et al, 20 Artyushkova and Fulghum, 21,22 Walton and Fairley, 23,24 and Smith, Briggs, and Fairley. 25 The image dataset was then processed using the CasaXPS software.…”

mentioning

confidence: 92%

Structure and growth of oxides on polycrystalline nickel surfaces

Payne

Grosvenor

Biesinger

et al. 2007

Surface & Interface Analysis

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The oxidation of polycrystalline nickel (Ni) metal surfaces after exposure to oxygen gas (O 2 ) at 25 and 300°C and pressures near 130 Pa, was studied using X-ray photoelectron spectroscopy (XPS). Oxide structures involving both divalent (Ni 2+ ) and trivalent (Ni 3+ ) species could be distinguished using Ni 2p spectra, while surface adsorbed O 2 and atomic oxygen (O) species could be differentiated from bulk oxide (O 2− ) using O 1s spectra. Oxide thicknesses and distributions were determined using QUASES  , and the average oxide thickness was verified using the Strohmeier formula. The reaction kinetics for oxide films grown at 300°C followed a parabolic mechanism, with an oxide thickness of greater than 4 nm having formed after 60 min. Exposure at 25°C followed a direct logarithmic mechanism with an oxide growth rate about four to five times slower than at 300°C. Reaction of a Ni (100) single crystal under comparable conditions showed much slower reaction rates compared to polycrystalline specimens. The higher reaction rate of the polycrystalline materials is attributed to grain boundary transport of Ni cations. Oxide thickness was measured on a microscopic scale for polycrystalline Ni exposed to large doses of O 2 at 25 and 300°C. The thickness of oxide was not strongly localized on this scale. However, the QUASES  analysis suggests that there is localized growth on a nanometric scale -the result of island formation. Copyright  2007 John Wiley & Sons, Ltd.KEYWORDS: X-ray photoelectron spectroscopy; nickel; oxidation; polycrystalline surfaces INTRODUCTIONThe oxidation of nickel (Ni) metal surfaces at ambient temperatures leads to the formation of thin passive films that tend to be described best using logarithmic kinetics. 1Following passivation there is little subsequent change in oxide thickness with time. 2 The mechanism is believed to follow that which was first suggested by Mott and Cabrera. 3 Reactant oxygen molecules (O 2 ) adsorb onto the surface of the metal and decompose into atomic oxygen (O (ads)). 4 The O (ads) then bonds covalently with the Ni metal atoms at the surface, weakening their attachment to the lattice. 4 Owing to the difference in electronegativity between Ni and O, a dipole forms which allows the two atoms to exchange places.4 Such a place exchange mechanism is responsible for the formation of the first one or two monolayers of oxide only. 4 Further oxidation is driven by the formation of an electric field created by the tunneling of electrons from the Ni atoms in the metal, through the thin oxide layer, to the O (ads) sitting on the surface. 1 The presence of this electric field induces the movement of ions through the oxide leading to the formation of a thicker film.1 After the film reaches a Ł Correspondence to: Brad P. Payne, Department of Chemistry, Room G-4, Western Science Centre, The University of Western Ontario, London, ON N6A 5B7, Canada. E-mail: bpayne2@uwo.ca certain thickness, the electric field is no longer strong enough to promote ion diffusion and oxidation sto...

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mentioning

confidence: 92%

Structure and growth of oxides on polycrystalline nickel surfaces

Payne

Grosvenor

Biesinger

et al. 2007

Surface & Interface Analysis

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“…Another set of complex surfaces was also studied by Barkshire et al 65 who examined both new and used surfaces of PtRh catalysts. This work was in collaboration with Ian Fletcher and David Briggs of ICI Research Laboratories.…”

Section: The Construction Of Mulsammentioning

confidence: 96%

From LEED to MULSAM

Prutton

2000

Surf. Interface Anal.

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This account gives an outline of the work done in the Department of Physics, University of York since 1965. The Surface Physics Group has been particularly active in the development and application of electron probes of solid surfaces with strong emphasis upon low‐energy electron diffraction and scanning electron microscopy using Auger electrons to form images. A scanning Auger microscope using multi‐imaging (MULSAM) has been particularly fruitful for the study of a variety of heterogeneous materials. Examples are given of the application of MULSAM to the minimization of topographic contrast artefacts, to the study of multilayers of magnetic materials, to the characterization of very rough PtRh catalyst surfaces, to the interpretation of the shapes of electron spectra and to the angular dependence of both Auger electron and energy‐dispersive x‐ray signals. Copyright © 2000 John Wiley & Sons, Ltd.

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“…In materials science, the method has found application to series of spectra that show variations (AES [22,23], XPS [23,24], EELS [25], EDX [26]), to sets of images [27] and in spectrochemical imaging, e. g., to methods capable of recording spectra at every point of an image (e. g., ToF-SIMS [28], Imaging XPS [21]). Programs for FA of electron spectra are commercially available (PHI Multipak [29], CASA XPS [30]).…”

Section: Multivariate Data Analysismentioning

confidence: 99%

Application of factor analysis in electron spectrometry (AES, XPS) for materials science

Baunack¹,

Oswald²

2005

MEKU

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Electron spectroscopic methods as X-ray photoelectron spectrometry (XPS) and Auger electron spectrometry (AES) are well established in the field of thin-film and surface analysis. In the measured spectral information, always also chemical information on the sample is contained. It is discussed that often chemometrical methods are the only way to extract such (hidden) information from the measured data sets. We demonstrate for AES and XPS measurements, how factor analysis (FA) can help to derive chemical information at Ti-based material developed for body implants. An introduction to the methodology is given, and challenges and restrictions are discussed.

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Quantitative surface microanalysis of samples with extreme topography utilising image interpretation by scatter diagrams and principal component analysis

Cited by 14 publications

References 18 publications

Structure and growth of oxides on polycrystalline nickel surfaces

Structure and growth of oxides on polycrystalline nickel surfaces

From LEED to MULSAM

Application of factor analysis in electron spectrometry (AES, XPS) for materials science

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