BS ISO 18118-2015 Surface chemical analysis Auger electron spectroscopy and X-ray photoelectron spectroscopy Guide to the use of experimentally determined relative sensitivity fact .pdf

1、BSI Standards PublicationBS ISO 18118:2015Surface chemical analysis Auger electron spectroscopyand X-ray photoelectronspectroscopy Guide tothe use of experimentallydetermined relative sensitivityfactors for the quantitativeanalysis of homogeneousmaterialsBS ISO 18118:2015 BRITISH STANDARDNational fo

2、rewordThis British Standard is the UK implementation of ISO 18118:2015. It supersedes BS ISO 18118:2004 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee CII/60, Surface chemical analysis.A list of organizations represented on this committee can be obtai

3、ned on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 87880 0ICS 71.040.40Compliance with

4、 a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 18118:2015 ISO 2015Surface chemic

5、al analysis Auger electron spectroscopy and X-ray photoelectron spectroscopy Guide to the use of experimentally determined relative sensitivity factors for the quantitative analysis of homogeneous materialsAnalyse chimique des surfaces Spectroscopie des lectrons Auger et spectroscopie de photolectro

6、ns Lignes directrices pour lutilisation de facteurs exprimentaux de sensibilit relative pour lanalyse quantitative de matriaux homognesINTERNATIONAL STANDARDISO18118Second edition2015-04-01Reference numberISO 18118:2015(E)BS ISO 18118:2015ISO 18118:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PRO

7、TECTED DOCUMENT ISO 2015All 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 written permission. Per

8、mission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 18118:2015ISO 18118:2

9、015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols and abbreviated terms . 25 General information . 36 Measurement conditions . 46.1 General . 46.2 Excitation source . 46.3 Energy resolution . 46.4 Energy step and scan rate 46.5 Signal intensity 46

10、6 Gain and time constant (for AES instruments with analogue detection systems) . 46.7 Modulation to generate a derivative spectrum . 47 Data-analysis procedures 58 Intensity-energy response function . 59 Determination of chemical composition using relative sensitivity factors . 59.1 Calculation of

11、chemical composition . 59.1.1 General 59.1.2 Composition determined from elemental relative sensitivity factors .69.1.3 Composition determined from atomic relative sensitivity factors or average matrix relative sensitivity factors 69.2 Uncertainties in calculated compositions 6Annex A (normative) Fo

12、rmulae for relative sensitivity factors 7Annex B (informative) Information on uncertainty of the analytical results .20Bibliography .23 ISO 2015 All rights reserved iiiContents PageBS ISO 18118:2015ISO 18118:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide feder

13、ation of national standards bodies (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 commit

14、tee. International organizations, governmental 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

15、those intended for its further maintenance 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

16、2 (see www.iso.org/directives).Attention 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

17、document will be in the Introduction 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

18、and expressions related to conformity 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 analysi

19、s, Subcommittee SC 7, Electron spectroscopies.This second edition cancels and replaces the first edition (ISO 18118:2004), which has been technically revised.iv ISO 2015 All rights reservedBS ISO 18118:2015ISO 18118:2015(E)IntroductionAuger electron spectroscopy (AES) and X-ray photoelectron spectro

20、scopy (XPS) are surface-analytical techniques that are sensitive to the composition in the surface region of a material to depths of, typically, a few nanometres (nm). Both techniques yield a surface-weighted signal, averaged over the analysis volume. Most samples have compositional variations, both

21、 laterally and with depth, and quantification is often performed with approximate methods since it can be difficult to determine the magnitude of any compositional variations and the distance scale over which they might occur. The simplest sample for analysis is one that is homogeneous. Although thi

22、s situation occurs infrequently, it is often assumed, for simplicity in the analysis, that the sample material of interest is homogeneous. This International Standard provides guidance on the measurement and use of experimentally determined relative sensitivity factors for the quantitative analysis

23、of homogeneous materials by AES and XPS. ISO 2015 All rights reserved vBS ISO 18118:2015BS ISO 18118:2015Surface chemical analysis Auger electron spectroscopy and X-ray photoelectron spectroscopy Guide to the use of experimentally determined relative sensitivity factors for the quantitative analysis

24、 of homogeneous materials1 ScopeThis International Standard gives guidance on the measurement and use of experimentally determined relative sensitivity factors for the quantitative analysis of homogeneous materials by Auger electron spectroscopy and X-ray photoelectron spectroscopy.2 Normative refer

25、encesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO

26、 18115, Surface chemical analysis VocabularyISO 21270, Surface chemical analysis X-ray photoelectron and Auger electron spectrometers Linearity of intensity scale3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 18115 and the following apply.3.1absolute

27、 elemental sensitivity factorcoefficient for an element by which the measured intensity for that element is divided to yield the atomic concentration or atomic fraction of the element present in the sampleNote 1 to entry: The choice of use of atomic concentration or atomic fraction should be made cl

28、ear.Note 2 to entry: The type of sensitivity factor used should be appropriate for the equations used in the quantification process and for the type of sample analysed, for example, of homogeneous samples or segregated layers.Note 3 to entry: The source of the sensitivity factors should be given in

29、order that the correct matrix factors or other parameters have been used.Note 4 to entry: Sensitivity factors depend on parameters of the excitation source, the spectrometer, and the orientation of the sample to these parts of the instrument. Sensitivity factors also depend on the matrix being analy

30、sed and in SIMS, this has a dominating influence.SOURCE: ISO 18115:2013, modified3.2relative elemental sensitivity factorcoefficient proportional to the absolute elemental sensitivity factor (3.1), where the constant of proportionality is chosen such that the value for a selected element and transit

31、ion is unityNote 1 to entry: Elements and transitions commonly used are C 1s or F 1s for XPS and Ag M4,5VV for AES.Note 2 to entry: The type of sensitivity factor used should be appropriate for the analysis, for example, of homogeneous samples or segregated layers.INTERNATIONAL STANDARD ISO 18118:20

32、15(E) ISO 2015 All rights reserved 1BS ISO 18118:2015ISO 18118:2015(E)Note 3 to entry: The source of the sensitivity factors should be given in order that the correct matrix factors or other parameters have been used.Note 4 to entry: Sensitivity factors depend on parameters of the excitation source,

33、 the spectrometer, and the orientation of the sample to these parts of the instrument. Sensitivity factors also depend on the matrix being analysed and in SIMS, this has a dominating influence.SOURCE: ISO 18115:20133.3average matrix relative sensitivity factorcoefficient proportional to the intensit

34、y calculated for a pure element in an average matrix with which the measured intensity for that element is divided in calculations to yield the atomic concentration or atomic fraction of the element present in the sampleNote 1 to entry: The choice of use of atomic concentration or atomic fraction sh

35、ould be made clear.Note 2 to entry: The type of sensitivity factor used should be appropriate for the equations used in the quantification process and for the type of sample analysed, for example, of homogeneous samples or segregated layers.Note 3 to entry: The source of the sensitivity factors shou

36、ld be given. Matrix factors are taken to be unity for average matrix relative sensitivity factors.Note 4 to entry: Sensitivity factors depend on parameters of the excitation source, the spectrometer, and the orientation of the sample to these parts of the instrument.SOURCE: ISO 18115:2013, modified3

37、4pure-element relative sensitivity factorcoefficient proportional to the intensity measured for a pure sample of an element with which the measured intensity for that element is divided in calculations to yield the atomic concentration or atomic fraction of the element present in the sampleNote 1 t

38、o entry: The choice of use of atomic concentration or atomic fraction should be made clear.Note 2 to entry: The type of sensitivity factor used should be appropriate for the equations used in the quantification process and for the type of sample analysed, for example, of homogeneous samples or segre

39、gated layers.Note 3 to entry: The source of the sensitivity factors should be given in order that the correct matrix factors or other parameters have been used. Matrix factors are significant and should be used with pure-element relative sensitivity factors.Note 4 to entry: Sensitivity factors depen

40、d on parameters of the excitation source, the spectrometer, and the orientation of the sample to these parts of the instrument.SOURCE: ISO 18115:2013, modified4 Symbols and abbreviated termsAES Auger electron spectroscopyAMRSF Average matrix relative sensitivity factorARSF Atomic relative sensitivit

41、y factorERSF Elemental relative sensitivity factorIERF Intensity-energy response functionSiAt Atomic relative sensitivity factor for element i2 ISO 2015 All rights reservedBS ISO 18118:2015ISO 18118:2015(E)SiAv Average matrix relative sensitivity factor for element iSiE Elemental relative sensitivit

42、y factor for element iRSF Relative sensitivity factorXPS X-ray photoelectron spectroscopy5 General informationIt is convenient in many quantitative applications of AES and XPS to utilize relative sensitivity factors (RSFs) for quantitative analyses. Three types of RSF have been used for this purpose

43、 elemental relative sensitivity factors (ERSFs), atomic relative sensitivity factors (ARSFs), and average matrix relative sensitivity factors (AMRSFs). Formulae defining these three types of RSF are given in A.3 and the principles on which these formulae are based on are given in A.2.While the ERSF

44、s are the simplest and easiest to apply, they are the least accurate because no account is taken of matrix correction factors (as described in A.3). The matrix correction factors for AES can vary between 0,1 and 81while they can vary between 0,3 and 32for XPS. The ARSFs are more accurate than ERSFs

45、in that they take account of differences in atomic densities, generally the largest single matrix correction. The AMRSFs are the most reliable RSFs in that there is almost complete correction of matrix effects. It is recommended that ERSFs be used only for semi-quantitative analyses (that is, rough

46、estimates of composition) and that ARSFs or preferably, AMRSFs be used for quantitative analyses. For the latter applications, ARSFs shall be used only in situations for which it is not possible to make use of AMRSFs (for example, measurements involving Auger electrons or photoelectrons at energies

47、for which inelastic mean free paths cannot be reliably determined).In analytical applications of AES and XPS, it is essential that Auger-electron and photoelectron intensities be measured using exactly the same procedure as that used for measurement of the RSFs. For some applications of AES (e.g. sp

48、utter depth profiles), it is convenient to use peak-to-peak heights of Auger-electron signals in the differential mode as measures of Auger-electron intensities. For other applications of AES (e.g. scanning Auger microscopy), the Auger-electron intensity can be determined from the difference between

49、 the intensity at a peak maximum in the direct spectrum and the intensity of a nearby background signal. Finally, for many applications in XPS and for some applications of AES, areas of peaks in direct spectra are used as measures of photoelectron or Auger-electron intensities.Relative sensitivity factors depend on the parameters of the excitation source (for example, the incident electron energy in AES and the choice of X-ray energy in XPS), the spectrometer configuration (for example, the angle of incidence of the electr