Summary of ISO/TC 201 Standard: XXIX. ISO 20903: 2006—Surface chemical analysis—Auger electron spectroscopy and X‐ray photoelectron spectroscopy—methods used to determine peak intensities and information required when reporting results

This article is a brief summary of the ISO Standard 20903. This standard provides information on methods for the measurement of peak intensities in Auger electron and X‐ray photoelectron spectra and on uncertainties of the derived peak areas. It also specifies the necessary information required in a report of analytical results based on such measurements. Published in 2007 by John Wiley & Sons, Ltd.     

Summary of ISO/TC201 technical report: ISO/TR 18392: 2005—Surface chemical analysis—X‐ray photoelectron spectroscopy—Procedures for determining backgrounds

ISO Technical Report 18392 provides the guidance for determining backgrounds in X‐ray photoelectron spectra. The methods of background determination described in this report are applicable for the quantitative evaluation of the spectra of photoelectrons and Auger electrons excited by X‐rays from solid surfaces and surface nanostructures. Copyright © 2006 John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 Technical Report: ISO/TR 19319: 2003—Surface chemical analysis—Auger electron spectroscopy and x‐ray photoelectron spectroscopy—Determination of lateral resolution,analysis area and sample area viewed by the analyser

ISO Technical Report 19319:2003 contains information on the determination of lateral resolution, analysis area and sample area viewed by the analyser in surface analyses by Auger electron spectroscopy and x‐ray photoelectron spectroscopy. This article provides a brief summary of this information. Copyright © 2004 John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 standard: XXI. ISO 21270:2004—Surface chemical analysis—X‐ray photoelectron and Auger electron spectrometers—Linearity of intensity scale

This International Standard specifies two methods for determining the maximum count rate for an acceptable limit of divergence from linearity of the intensity scale of Auger and x‐ray photoelectron spectrometers. It also includes methods to correct for intensity non‐linearities so that a higher maximum count rate can be employed for those spectrometers for which the relevant correction equations have been shown to be valid. Copyright © 2004 John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 Standard: XXX. ISO 18516: 2006—Surface chemical analysis—Auger electron spectroscopy and X‐ray photoelectron spectroscopy—Determination of lateral resolution

This International Standard describes three methods for measuring the lateral resolution achievable in Auger electron spectrometers and X‐ray photoelectron spectrometers under defined settings. The straight‐edge method is suitable for instruments where the lateral resolution is expected to be larger than 1 µm. The grid method is suitable if the lateral resolution is expected to be less than 1 µm but more than 20 nm. The gold‐island method is suitable for instruments where the lateral resolution is expected to be less than 50 nm. The standard contains three informative annexes that provide illustrative examples of measurements of lateral resolution. Copyright © 2008 John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 standard: XVIII,ISO 19318:2004—surface chemical analysis—X‐ray photoelectron spectroscopy—Reporting of methods used for charge control and charge correction

International Standard ISO 19318 specifies the minimum amount of information describing the methods of charge control and charge correction in measurements of core‐level binding energies for insulating specimens by x‐ray photoelectron spectroscopy, which is to be reported with the analytical results. Information is also provided on methods that have been found useful for charge control and charge correction in the measurement of binding energies. Copyright © 2005 John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 Standard: ISO 14701:2011 – Surface chemical analysis – X‐ray photoelectron spectroscopy—measurement of silicon oxide thickness

This International Standard specifies several methods for measuring the oxide thickness at the surfaces of (100) and (111) silicon wafers as an equivalent thickness of silicon dioxide when measured using X‐ray photoelectron spectroscopy. It is only applicable to flat, polished samples and for instruments that incorporate an Al or Mg X‐ray source, a sample stage that permits defined photoelectron emission angles and a spectrometer with an input lens that may be restricted to less than a 6° cone semiangle. For thermal oxides in the range 1‐ to 8‐nm thickness, using the best method described in this International Standard, uncertainties at a 95% confidence level around 2% may be typical and around 1% at optimum. A simpler method is also given with slightly poorer, but often adequate, uncertainties. Copyright © 2012 Crown copyright.     

Summary of ISO/TC201 standard: ISO/TR 18394:2006—surface chemical analysis—Auger electron spectroscopy—derivation of chemical information

ISO/TR 18394 provides guidance for the identification of chemical effects on x‐ray or electron‐excited Auger electron spectra as well as for applications of these effects in chemical characterization of surface/interface layers of solids. In addition to elemental composition, information can be obtained on the chemical state and the surrounding local electronic structure of the atom with the initial core hole from the changes of Auger electron spectra upon the alteration of its local environment. The methods of identification and use of chemical effects on Auger electron spectra, as described in this Technical Report, are very important for accurate quantitative applications of Auger electron spectroscopy. Copyright © 2007 John Wiley & Sons, Ltd.     

Interlaboratory study comparing analyses of simulated angle‐resolved X‐ray photoelectron spectroscopy data

An interlaboratory study has been conducted to determine the following: (i) the similarities and differences of film thicknesses and composition profiles obtained from analyses of simulated angle‐resolved X‐ray photoelectron spectroscopy (ARXPS) data by different analysts using different algorithms for data analysis, and (ii) the effects of two assumptions commonly made in data‐analysis algorithms for ARXPS on derived film thicknesses and composition profiles. The analyzed data were generated by the National Institute of Standards and Technology Database for the Simulation of Electron Spectra for Surface Analysis, (SESSA) which provides a simple way to study the influence of the aforementioned effects on compositional depth profile reconstruction. Sets of simulated ARXPS data were produced for thin films of SiO₂, SiON, HfO₂, and HfON of varying thicknesses on a Si substrate. For some HfON films, the N concentration varied with depth. Eleven groups participated in the round robin study. The majority (eight) employed a commercial ARXPS instrument in which the angular distribution is measured for a fixed sample geometry, in contrast to conventional ARXPS in which the sample is tilted for angular variation. The average deviations between the reported average depth, film thickness, and amount of material typically varied between 20% and 30% but were considerably larger, between 30% and 80%, for some cases. The average errors were generally larger for simulations that included elastic scattering and the finite analyzer‐acceptance angle (realistic conditions) than those for simulations that neglected elastic scattering and the finite analyzer‐acceptance angle (simplified conditions). The retrieved N depth profiles were quantitatively different from the true depth profiles and showed substantial variability among the group of members who used the same instrument and analysis software. Copyright © 2014 John Wiley & Sons, Ltd.     

X‐ray photoelectron spectroscopy and the pattern recognition method—their application to surface studies in CoPd alloys

In the present work, polycrystalline CoPd alloys in varying range of bulk atomic percent composition (Co30Pd70, Co50Pd50 and Co70Pd30) are investigated by means of X‐ray photoelectron spectroscopy (XPS). The results of conventional XPS quantitative multiline (ML) approach are compared to the results obtained on the basis of XPS lines shape analysis, where the selected XPS or X‐ray induced Auger electron (XAES) transitions, are processed using the pattern recognition method known as the fuzzy k‐nearest neighbour (fkNN) rule. The fkNN rule is applied to the following spectra line shapes: Pd MNV, Co 2p, Co LMM, Pd 3d and valence band, analysing electrons in a varying range of selected kinetic energies. Both methods showed the surface segregation of Pd in Co30Pd70 and Co50Pd50 alloys. The results of the ML, the binding energy shift (ΔBE) analysis and the fkNN rule remained in agreement. Discrepancies in quantitative results obtained using different approaches are discussed within the accuracy of the applied methods, differences due to mean escape depth (MED) of electrons in considered transitions, their depth distribution function, the sensitivity of electron transition line shape on the environmental change (weaker effect for the inner shell transitions, and stronger effect for the outer shell transitions and Auger electron spectroscopy (AES) electrons transitions) and the non‐uniform depth profile concentrations. Copyright © 2005 John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 Standard XII. ISO 17973:2002—Surface chemical analysis—Medium‐resolution Auger electron spectrometers—Calibration of energy scales for elemental analysis

This International Standard specifies a method for calibrating the kinetic energy scale of Auger electron spectrometers with an uncertainty of 3 eV for general analytical use for identifying elements at surfaces. It is suitable for instruments used in either the direct mode or the differential mode where the resolution is equal to or less than 0.5% and the modulation amplitude for the differential mode, if used, is 2 eV peak to peak. The spectrometer shall be equipped with an inert gas ion gun or other method for sample cleaning and with an electron gun capable of operating at 4 keV or higher beam energy. This International Standard further specifies a calibration schedule. Crown Copyright © 2003. Published by John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 Standard XI. ISO 17974:2002—Surface chemical analysis—High‐resolution Auger electron spectrometers—Calibration of energy scales for elemental and chemical‐state analysis

This International Standard specifies a method for calibrating the kinetic energy scales of Auger electron spectrometers for elemental and chemical‐state analysis at surfaces. It is only applicable to instruments that incorporate an ion gun for sputter cleaning. This International Standard further specifies a method to establish a calibration schedule, to test for the kinetic energy scale linearity at one intermediate energy, to confirm the uncertainty of the scale calibration at one low and one high kinetic energy value, to correct for small drifts of that scale and to define the expanded uncertainty of the calibration of the kinetic energy scale for a confidence level of 95%. This uncertainty includes contributions for behaviours observed in interlaboratory studies but does not cover all of the defects that could occur. This International Standard is not applicable to instruments with kinetic energy scale errors that are significantly non‐linear with energy, to instruments operated at relative resolutions poorer than 0.2% in the constant ΔE/E mode or poorer than 1.5 eV in the constant ΔE mode, to instruments requiring tolerance limits of ±0.05 eV or less or to instruments equipped with an electron gun that cannot be operated in the energy range 5–10 keV. This standard does not provide a full calibration check, which would confirm the energy measured at each addressable point on the energy scale and should be performed according to the manufacturer's recommended procedures. Crown Copyright © 2003. Published by John Wiley & Sons, Ltd.     

Summary of ISO/TC 201 Standard: ISO 18115‐1:2010 – surface chemical analysis – vocabulary – general terms and terms used in spectroscopy

This International Standard revises ISO 18115:2001 and the two subsequent amendments by bringing the material up to date and separating out the general terms and terms used in spectroscopy into Part 1, and terms relating to scanning probe microscopy into Part 2. This part, Part 1, covers 548 terms used in Auger electron spectroscopy, elastic peak electron spectroscopy, reflected electron energy loss spectroscopy, secondary ion mass spectrometry, ultra‐violet photoelectron spectroscopy, X‐ray photoelectron spectroscopy, and so on, as well as 52 acronyms. The terms cover words or phrases used in describing the samples, instruments, and theoretical concepts involved in surface chemical analysis. Copyright © 2012 Crown copyright.     

Summary of ISO/TC 201 Standard: ISO 18115‐1:2013 – Surface chemical analysis – Vocabulary – General terms and terms used in spectroscopy

Amendments have been made to International Standards Organization (ISO) 18115‐1:2010 extending the number of terms and, in a few cases where usage has changed, incorporating revisions. Part 1 covers 600 terms used in Auger electron spectroscopy, elastic peak electron spectroscopy, reflected electron energy loss spectroscopy, SIMS, UPS, XPS, etc. as well as 75 acronyms. The terms cover words or phrases used in describing the samples, instruments and theoretical concepts involved in surface chemical analysis. © 2014 Crown copyright. Surface and Interface Analysis © 2014 John Wiley & Sons, Ltd.     

Surface oxidation process of a diamond‐like carbon film analyzed by difference X‐ray photoelectron spectroscopy

Difference X‐ray photoelectron spectroscopy (D‐XPS) revealed the surface oxidation process of a diamond‐like carbon (DLC) film. Evaluation of surface functional groups on DLC solely by the C 1s spectrum is difficult because the spectrum is broad and has a secondary asymmetric lineshape. D‐XPS clarified the subtle but critical changes at the DLC surface caused by wet oxidation. The hydroxyl (C―OH) group was dominant at the oxidized surface. Further oxidized carbonyl (C?O) and carboxyl (including carboxylate) (COO) groups were also obtained; however, the oxidation of C?O to COO was suppressed to some extent because the reaction required C―C bond cleavage. Wet oxidation cleaved the aliphatic hydrogenated and non‐hydrogenated sp² carbon bonds (C―H sp² and C―C sp²) to create a pair of C―OH and hydrogenated sp³ carbon (C―H sp³) bonds. The reaction yield for C―H sp² was superior at the surface, suggesting that the DLC film was hydrogen rich at the surface. Oxidation of aromatic sp² rings or polycyclic aromatic hydrocarbons such as nanographite to phenols did not occur because of their resonance stabilization with electron delocalization. Non‐hydrogenated sp³ carbon (C―C sp³) bonds were not affected by oxidation, suggesting that these bonds are chemically inert. Copyright © 2014 John Wiley & Sons, Ltd.     

Application of surface analysis methods to nanomaterials: summary of ISO/TC 201 technical report: ISO 14187:2011 – surface chemical analysis – characterization of nanomaterials

The ISO technical report 14187 provides an introduction to (and examples of) the information that can be obtained about nanostructured materials by using surface analysis tools. In addition, both general issues and challenges associated with characterizing nanostructured materials and the specific opportunities and challenges associated with individual analytical methods are identified. As the size of objects or components of materials approaches a few nanometers, the distinctions among ‘bulk’, ‘surface’, and ‘particle’ analysis blur. This technical report focuses on issues specifically relevant to surface chemical analysis of nanostructured materials. The report considers a variety of analysis methods but focuses on techniques that are in the domain of ISO/TC 201 including Auger electron spectroscopy, X‐ray photoelectron spectroscopy, secondary ion mass spectrometry, and scanning probe microscopy. Measurements of nanoparticle surface properties such as surface potential that are often made in a solution are not discussed. Copyright © 2012 John Wiley & Sons, Ltd.     

Quantitative analysis of trace levels of surface contamination by X‐ray photoelectron spectroscopy. Part II: Systematic uncertainties and absolute quantification

We discuss analyses of trace levels of surface contamination using X‐ray photoelectron spectroscopy (XPS). The problem of quantifying common sources of statistical and systematic uncertainties for these measurements is formulated in terms of the needs of extreme ultraviolet lithography, but the results and conclusions are applicable to a broad range of XPS applications. We quantify the systematic uncertainties introduced by particular cases of overlapping peaks on different substrate structures by simulating measured spectra with the National Institute of Standards and Technology Database for the Simulation of Electron Spectra for Surface Analysis (SESSA). One example demonstrates that the relative atomic concentrations of trace elements such as S, P, and halogens on a Ru surface could be dramatically overestimated if the fitting of the overlapping Ru 3d and C 1s peaks excludes the contribution from carbon. We also show how spectra generated by SESSA can be compared with measured spectra to determine absolute amounts of surface impurities on layered samples of the type used for extreme ultraviolet lithography. We provide estimates of the total uncertainty for such measurements by considering the systematic limitations of SESSA and the statistical uncertainties of the measurements. The same procedure can be employed for other multilayered materials. Finally, we describe two approaches for converting XPS detection limits for an elemental impurity in an elemental matrix to the corresponding detection limits for the impurity as a thin film on the surface of the matrix material.     

Quantitative analysis of trace levels of surface contamination by X‐ray photoelectron spectroscopy. Part I: Statistical uncertainty near the detection limit

We discuss the problem of quantifying common sources of statistical uncertainties for analyses of trace levels of surface contamination by using X‐ray photoelectron spectroscopy. We examine the propagation of error for peak‐area measurements by using common forms of linear and polynomial background subtraction including the correlation of points used to determine both background and peak areas. This correlation has been neglected in previous analyses, but we show that it contributes significantly to the peak‐area uncertainty near the detection limit. We introduce the concept of relative background subtraction variance (RBSV) that quantifies the uncertainty introduced by the method of background determination relative to the uncertainty of the background area itself. The uncertainties of the peak area and atomic concentration and of the detection limit are expressed using the RBSV, which separates the contributions from the acquisition parameters, the background‐determination method, and the properties of the measured spectrum. These results are then combined to find acquisition strategies that minimize the total measurement time needed to achieve a desired detection limit or atomic‐percentage uncertainty for a particular trace element. Minimization of data‐acquisition time is important for samples that are sensitive to X‐ray dose and also for laboratories that need to optimize throughput.     

Summary of ISO/TC 201 standard: ISO 19668—Surface chemical analysis—X‐ray photoelectron spectroscopy—Estimating and reporting detection limits for elements in homogeneous materials

This International Standard specifies a procedure by which elemental detection limits in X‐ray photoelectron spectroscopy (XPS) can be estimated from data for a particular sample in common analytical situations and reported. This document is applicable to homogeneous materials and is not applicable if the depth distribution of elements is inhomogeneous within the information depth of the technique.     

Improving surface‐analysis methods for characterization of advanced materials by development of standards,reference data,and interlaboratory comparisons

This paper summarizes the results of two surveys examining current needs for improved analyses of surfaces. Surfaces and interfaces are increasingly important to science and technologies associated with nanoparticles, nano‐structured materials and other complex materials including those associated with information systems and medical or biological applications. Adequate characterization of advanced materials frequently requires application of more than one analysis method along with the need to analyze data in increasingly sophisticated and sometimes interrelated ways. It is useful for both new and experienced analysts to have ready access to best practices for obtaining accurate and useful information from a variety of different analysis tools. The International Organization for Standardization (ISO) Committee TC 201 on surface chemical analysis and the ASTM Committee E‐42 on surface analysis are working to address these needs by assembling guides and standards reflecting the collective experience and wisdom of experts in this community. Published in 2007 by John Wiley & Sons, Ltd