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Title: Module to guide the expert use of x-ray photoelectron spectroscopy by corrosion scientists

Abstract

This contribution, to the potential development of data systems having some degree of 'expert' character for use in x-ray photoelectron spectroscopy (XPS), illustrates the manner in which models of 'Rules' might be developed by the user community. The field of corrosion science is taken as an example of one community of researchers who make regular use of XPS for well defined needs. These 'needs' are redefined as a series of Goals that have to be reached in order to characterize the surface in terms of layer sequences and the enrichment of given elements within them. Rules are written to allow a structured approach to achieve each Goal. A feature of this set of Rules is that they are designed expressly to allow automated interpretation of the survey scan. This approach is facilitated by the use of a recommendation that the survey spectrum be acquired as a series of accumulated scans instead of the usual approach of making a single scan through the spectrum. Repeat scans enable the information extracted by the operation of the Rules to be processed and displayed for information during the period that is normally used for the survey scan. It is intended that this information willmore » inform the setting up of any subsequent high resolution scans and their interactive interpretation. It will also inform any future operations such as ion etching or angle-resolved measurements. In some cases, the information made available may be all that is required by the user and in this case the 'expert module' approach becomes particularly cost effective. The operation of the rules is illustrated throughout by an examination of data obtained for passivated stainless steel, giving a data set of measurements, typical of those made by corrosion scientists, that can be compared with the literature values obtained by more conventional XPS interpretation.« less

Authors:
 [1]
  1. Surface Analysis Laboratory, School of Engineering, Mail Drop H6, University of Surrey, Guildford GU2 7XH (United Kingdom)
Publication Date:
OSTI Identifier:
20853946
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Vacuum Science and Technology. A, International Journal Devoted to Vacuum, Surfaces, and Films; Journal Volume: 25; Journal Issue: 1; Other Information: DOI: 10.1116/1.2406058; (c) 2007 American Vacuum Society; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; CORROSION; ETCHING; SPECTRA; STAINLESS STEELS; SURFACES; X-RAY PHOTOELECTRON SPECTROSCOPY; X-RAY SPECTROSCOPY

Citation Formats

Castle, J. E. Module to guide the expert use of x-ray photoelectron spectroscopy by corrosion scientists. United States: N. p., 2007. Web. doi:10.1116/1.2406058.
Castle, J. E. Module to guide the expert use of x-ray photoelectron spectroscopy by corrosion scientists. United States. doi:10.1116/1.2406058.
Castle, J. E. Mon . "Module to guide the expert use of x-ray photoelectron spectroscopy by corrosion scientists". United States. doi:10.1116/1.2406058.
@article{osti_20853946,
title = {Module to guide the expert use of x-ray photoelectron spectroscopy by corrosion scientists},
author = {Castle, J. E.},
abstractNote = {This contribution, to the potential development of data systems having some degree of 'expert' character for use in x-ray photoelectron spectroscopy (XPS), illustrates the manner in which models of 'Rules' might be developed by the user community. The field of corrosion science is taken as an example of one community of researchers who make regular use of XPS for well defined needs. These 'needs' are redefined as a series of Goals that have to be reached in order to characterize the surface in terms of layer sequences and the enrichment of given elements within them. Rules are written to allow a structured approach to achieve each Goal. A feature of this set of Rules is that they are designed expressly to allow automated interpretation of the survey scan. This approach is facilitated by the use of a recommendation that the survey spectrum be acquired as a series of accumulated scans instead of the usual approach of making a single scan through the spectrum. Repeat scans enable the information extracted by the operation of the Rules to be processed and displayed for information during the period that is normally used for the survey scan. It is intended that this information will inform the setting up of any subsequent high resolution scans and their interactive interpretation. It will also inform any future operations such as ion etching or angle-resolved measurements. In some cases, the information made available may be all that is required by the user and in this case the 'expert module' approach becomes particularly cost effective. The operation of the rules is illustrated throughout by an examination of data obtained for passivated stainless steel, giving a data set of measurements, typical of those made by corrosion scientists, that can be compared with the literature values obtained by more conventional XPS interpretation.},
doi = {10.1116/1.2406058},
journal = {Journal of Vacuum Science and Technology. A, International Journal Devoted to Vacuum, Surfaces, and Films},
number = 1,
volume = 25,
place = {United States},
year = {Mon Jan 15 00:00:00 EST 2007},
month = {Mon Jan 15 00:00:00 EST 2007}
}
  • Surface analysis of the corrosion products formed on iron metal exposed to off gas from a HCN production process has been performed. The atmosphere contains HCN(g), NH/sub 3/(g), and H/sub 2/O(g) plus other trace gases. Iron gratings exposed to the atmosphere form a dark blue coating which pits the surface of the iron. Samples of the corroded iron surface were analyzed by FT-IR/photoacoustic spectroscopy (PAS) and x-ray photoelectron spectroscopy (XPS or ESCA). The mid-IR spectrum from PAS yielded peaks due to NH/sub 4/ /sup +/, CN/sup -/, and H/sub 2/O. ESCA analysis confirmed that the surface iron was divalent, coordinatedmore » to cyanide, and no iron(II) oxide was present. Relative quantitation from ESCA showed a 1:4 ratio of NH/sub 4//CN type nitrogen, thus a specific single stoichiometry was not postulated for the corrosion product. Peak positions of the cyanide stretching frequencies suggest a mixed ferro(ferrocyanide) complex, with some ammonium as a counterion. This study illustrates the detailed structural information obtainable from FT-IR/PAS with ESCA and the applicability of FT-IR/PAS to corrosion problems.« less
  • An updated version of the ASTM guide E1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to include new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997.
  • An updated version of the American Society for Testing and Materials (ASTM) guide E 1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM [Annual Book of ASTM Standards Surface Analysis (American Society for Testing and Materials, West Conshohocken, PA, 2004), Vol. 03.06]. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to includemore » new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997 [D. R. Baer and K. D. Bomben, J. Vac. Sci. Technol. A 16, 754 (1998)].« less
  • The localized orbital ionization potential (LOIP), involving both core and valence ionization potentials, is a valuable aid in the assignment of valence-photoelectron spectra. Its primary value is to provide chemists with a reliable method for interpreting valence-shell ionization potentials in terms of the bonding or antibonding character of molecular orbitals. Typical applications are the determination of the degree of interaction of so-called lone-pair orbitals (mainly consisting of p or d orbitals) either with filled orbitals (bond breaking orbitals or other lone pairs) or with empty orbitals (antibonding orbitals or higher energy d orbitals). This method allows chemists to make thesemore » interpretations using only experimental data, free from most of the calculational problems and interpretive ambiguities associated with theoretical methods. 2 figures, 8 tables.« less
  • A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutionsmore » and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II ╬▒ lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.« less