1、BSI Standards PublicationBS ISO 19830:2015Surface chemical analysis Electron spectroscopies Minimum reportingrequirements for peak fittingin X-ray photoelectronspectroscopyBS ISO 19830:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 19830:2015. The UK part
2、icipation in its preparation was entrusted to Technical Committee CII/60, Surface chemical analysis.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are res
3、ponsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 86519 0 ICS 71.040.40 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Sta
4、ndards Policy and Strategy Committee on 30 November 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 19830:2015 ISO 2015Surface chemical analysis Electron spectroscopies Minimum reporting requirements for peak fitting in X-ray photoelectron spectroscopyAnalyse ch
5、imique des surfaces Spectroscopie dlectrons Exigences minimales pour le rapport dajustement de pic en spectroscopie de photolectrons XINTERNATIONAL STANDARDISO19830First edition2015-11-15Reference numberISO 19830:2015(E)BS ISO 19830:2015ISO 19830:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTE
6、CTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
7、 written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 19830
8、:2015ISO 19830:2015(E)Foreword vIntroduction vi1 Scope . 12 Terms and definitions . 13 Symbols and abbreviated terms . 23.1 Abbreviated terms . 23.2 Symbols . 24 Reporting of relevant data acquisition parameters . 34.1 General . 34.2 Spectrometer 34.3 Instrument resolution. 34.4 Detector . 34.5 X-ra
9、y source . 44.6 Element identity 44.7 Energy range in the spectrum 44.8 Energy step size in spectrum 44.9 Charge compensation 45 Reporting of single-spectrum peak-fitting parameters . 55.1 General . 55.2 Background range 55.3 Background integration range . 55.4 Background type . 55.5 Application of
10、a fitted background 55.6 Setting the peak parameters . 65.7 Peak area and peak height 65.8 Peak area and peak height ratios 65.9 Full width at half maximum . 65.10 Peak shape 65.11 Peak asymmetry parameters 75.12 The peak-fitting process . 75.13 Residual spectrum . 76 Multi-spectrum peak fitting 76.
11、1 General . 76.2 Peak fitting methods for multi-spectrum data sets . 76.3 Propagation of constraints . 86.4 Background propagation 87 Satellite subtraction 98 Doublet subtraction 99 Spectrum deconvolution .1010 Fit quality and uncertainties .1010.1 General 1010.2 Fit quality 1010.3 Uncertainty in th
12、e reported binding energies 1010.4 Uncertainty in the peak areas . 10Annex A (informative) Example of reporting peak fitting .11Annex B (informative) Reporting peak fitting for multi-level data sets .14Annex C (informative) Template for reporting peak fitting parameters .17Annex D (informative) Stat
13、istical methods .19 ISO 2015 All rights reserved iiiContents PageBS ISO 19830:2015ISO 19830:2015(E)Bibliography .22iv ISO 2015 All rights reservedBS ISO 19830:2015ISO 19830:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
14、(ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, g
15、overnmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further main
16、tenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Atte
17、ntion is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introductio
18、n and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformi
19、ty assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information.The committee responsible for this document is ISO/TC 201, Surface chemical analysis, Subcommittee SC 7, Electron spec
20、troscopies. ISO 2015 All rights reserved vBS ISO 19830:2015ISO 19830:2015(E)IntroductionX-ray photoelectron spectra produced from the surfaces of many materials are complex and frequently consist of overlapping or unresolved peaks. The lack of resolution can be due to instrumental parameters, the X-
21、ray line width, the natural line width of the transition, or a contribution from all of these. It is frequently necessary, therefore, to use a mathematical procedure to fit some or all of the peaks in XPS spectra in order to establish the position and intensity of each of the component peaks contain
22、ed within each peak envelope. This is often the first step in the identification of the chemical states which give rise to the overall peak envelope and the quantification of each chemical state present. The analyst must therefore have confidence in both the position (to establish the chemical state
23、) and the peak area (to allow accurate quantification) of each peak reported following peak fitting.The mathematical procedure applies model peak and background shapes, the defining parameters of which are varied in order to obtain the optimum fit to the experimental data. Most commonly, the model p
24、eak shapes are some combination of Gaussian and Lorentzian functions.Many of the parameters that should be reported following peak fitting are those that define these curves. Other factors are those which are selected by the analyst to ensure that the peak-fitting process results in a chemically mea
25、ningful description of the peak envelope or to minimize the time taken for the fitting process. These include parameters that the analyst chooses to fix at a constant value during the fitting process, defines as a range of values over which the parameter can vary during the fitting process, and math
26、ematically links the value of a parameter to that of another parameterPeak fitting is a purely mathematical process from which quantitative and qualitative results are obtained which may be related to the chemistry of the surface being analysed. The results will depend upon the analysts choice of pa
27、rameters and constraints and this choice will influence the interpretive conclusions that the analyst reaches from the peak-fitting results. For that reason, it is important that these parameters and constraints are reported. This will allow another analyst to assess the reliability and validity of
28、the conclusions drawn from the peak fitting exercise, repeat the peak-fitting process on the same data set and obtain the same results, and repeat the peak-fitting process on data which has been obtained from a similar sample and be in a position to make a valid comparison of the data sets.Most soft
29、ware packages which have been designed for use with XPS data contain a peak-fitting routine. These routines allow the operator to select appropriate parameters and apply the desired constraints to the fitting process. It is highly likely that the software will provide an output which reports these a
30、nd usually includes the facility to copy them for use with another spectrum. Such an output will make reporting the appropriate parameters particularly convenient.This International Standard is not intended to provide instructions for either fitting XPS peaks or for linking the outcome of a peak-fit
31、ting routine to the chemistry of the surface being analysed. Indeed, in the examples shown in this International Standard, it is not claimed that the fitting shown is the only way fitting can be done or even that the examples show the optimum peak fitting method. The examples serve to illustrate the
32、 purpose of this International Standard.vi ISO 2015 All rights reservedBS ISO 19830:2015Surface chemical analysis Electron spectroscopies Minimum reporting requirements for peak fitting in X-ray photoelectron spectroscopy1 ScopeThe purpose of this International Standard is to define how peak fitting
33、 and the results of peak fitting in X-ray photoelectron spectroscopy shall be reported. It is applicable to the fitting of a single spectrum or to a set of related spectra, as might be acquired, for example, during a depth profile measurement. This International Standard provides a list of those par
34、ameters which shall be reported if either reproducible peak fitting is to be achieved or a number of spectra are to be fitted and the fitted spectra compared. This International Standard does not provide instructions for peak fitting nor the procedures which should be adopted.2 Terms and definitions
35、For the purposes of this document, the following terms and definitions apply.2.1background, inelasticintensity distribution in the spectrum for particles originally at one energy but which are emitted at lower energies due to one or more inelastic scattering processesSOURCE: ISO 18115-1, 4.502.2back
36、ground, Shirleybackground calculated to fit the measured spectrum at points at higher and lower kinetic energy than the peak or peaks of interest such that the background contribution at a given kinetic energy is in a fixed proportion to the total peak area above that background for higher kinetic e
37、nergies.SOURCE: ISO 18115-1:2010, 4.542.3background, Tougaardintensity distribution obtained from a model for the differential inelastic scattering cross section with respect to energy loss and the three-dimensional distribution of the emitting atoms in the surface regionSOURCE: ISO 18115-1:2010, 4.
38、572.4pass energymean kinetic energy of the detected particles in the energy dispersive portion of the energy analyserSOURCE: ISO 18115-1:2010, 4.3252.5peak fittingprocedure whereby a spectrum, generated by peak synthesis, is adjusted to match a measured spectrumINTERNATIONAL STANDARD ISO 19830:2015(
39、E) ISO 2015 All rights reserved 1BS ISO 19830:2015ISO 19830:2015(E)2.6peak synthesisprocedure whereby a synthetic spectrum is generated using either model or experimental peak shapes in which the number of peaks, peak shapes, peak widths, peak positions, peak intensities, and background shape and in
40、tensity are adjusted for peak fittingSOURCE: ISO 18115-1:2010, 4.3292.7residual spectrumdifference between the experimentally acquired spectrum and the synthesized spectrum3 Symbols and abbreviated terms3.1 Abbreviated termsBE binding energyeV electron voltFWHM full width at half maximumL/G ratio of
41、 the intensity of the Lorentzian component to the Gaussian component of a pseudo Voigt peak consisting of the sum of a Gaussian and a Lorentzian functionPE pass energyXPS X-ray photoelectron spectroscopy3.2 Symbolsmin2value of 2after the minimization process has been completed2chi squareastandard de
42、viation for the binding energy of a peakcitotal number of counts in channel i prior to background subtractioni channel number in a spectrumM number of independently adjustable parameters used in the fitting processN number of energy channels in the part of the spectrum being fittedrispectrum residua
43、l in channel i (obtained from the total number of counts, not counts per sec-ond)a energy by which a peak position is changed (from the position which results in the minimum chi square value) during the process of estimating the uncertainty in the peak positionh amount by which a peak height is chan
44、ged (from the value which results in the minimum chi square value) during the process of estimating the uncertainty in the peak intensityw amount by which a peak width is changed (from the value which results in the minimum chi square value) during the process of estimating the uncertainty in the pe
45、ak width2 ISO 2015 All rights reservedBS ISO 19830:2015ISO 19830:2015(E)4 Reporting of relevant data acquisition parameters4.1 GeneralThis Clause applies to the instrumental parameters that can affect the shape of a peak, peak envelope, or background in a spectrum. Such parameters will therefore aff
46、ect the parameters that define the fitted spectrum and so they shall be reported.4.2 SpectrometerThere are instrumental and acquisition parameters that influence the shape of the peaks in an XPS spectrum. These parameters can also affect the results of any peak fitting activity and shall be reported
47、.In addition, the relationship between instrumental parameters and the results obtained from peak fitting may depend upon the precise design of instrument used. An example of this is the relationship between the pass energy used to acquire the data and the resolution of the peaks in the spectrum. It
48、 is therefore necessary to report the manufacturer and the model of the instrumentation used. This can either be the model name (including a version identifier, if appropriate) of the complete spectrometer or the model names of the key components.4.3 Instrument resolutionThe parameters that can affe
49、ct the results of a subsequent peak fitting shall be reported. These include any of the following factors which can affect the resolution of the spectrometer: chosen pass energy; if the spectrometer has adjustable slits which control instrument resolution at the entrance and/or exit of the analyser, the settings for those slits; if the spectrometer has a transfer lens having an adjustable angular acceptance and/or an adjustable field of view aperture, the settings of each of these can affect the resulting resolution
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