1、BS ISO 15470:2017Surface chemical analysis X-ray photoelectron spectroscopy Description of selectedinstrumental performanceparametersBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 15470:2017 BRITISH STANDARDNational forewordThis British Standard is the UK imp
2、lementation of ISO 15470:2017. It supersedes BS ISO 15470:2004.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 obtained on request to its secretary.This publication does not pu
3、rport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 95233 3 ICS 71.040.40 Compliance with a British Standard cannot confer immunity from legal obli
4、gations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 15470:2017 ISO 2017Surface chemical analysis X-ray photoelectron spectroscopy Description o
5、f selected instrumental performance parametersAnalyse chimique des surfaces Spectroscopie de photolectrons X Description de certains paramtres relatifs la performance instrumentaleINTERNATIONAL STANDARDISO15470Second edition2017-03Reference numberISO 15470:2017(E)BS ISO 15470:2017ISO 15470:2017(E)ii
6、 ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, 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 o
7、n the internet or an intranet, without prior 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
8、09 47copyrightiso.orgwww.iso.orgBS ISO 15470:2017ISO 15470:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Abbreviated terms 15 Description of selected instrumental performance parameters . 15.1 Method of analysis . 15.2 Samples . 15.3 System configura
9、tion . 25.4 X-ray source . 25.4.1 Anode type 25.4.2 Anode power . 25.4.3 Expected anode lifetime 25.5 Spectrometer intensity performance and energy resolution . 25.6 Spectrometer energy scale . 25.7 Spectrometer intensity linearity 35.8 Spectrometer response function . 35.9 Imaging and selected area
10、 resolution . 35.9.1 General 35.9.2 Method 1 . 35.9.3 Method 2 . 35.9.4 Method 3 . 45.10 Charge neutralization 45.11 Angle-resolved XPS 45.12 Vacuum environment 4Bibliography 5 ISO 2017 All rights reserved iiiContents PageBS ISO 15470:2017ISO 15470:2017(E)ForewordISO (the International Organization
11、for Standardization) is a worldwide federation 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 t
12、he right to be represented on that committee. 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 proc
13、edures used to develop this document and 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 editori
14、al rules of the ISO/IEC Directives, Part 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 righ
15、ts identified during the development of the 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 ex
16、planation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .o
17、rg/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 7, X-ray photoelectron spectroscopy. This second edition cancels and replaces the first edition (ISO 15470:2004), of which it constitutes a minor revision.The changes comp
18、ared to the previous edition are as follows: a typo has been corrected in 5.10; a Bibliography has been added; the text has been editorially revised to comply with the most recent drafting rules.iv ISO 2017 All rights reservedBS ISO 15470:2017ISO 15470:2017(E)IntroductionX-ray photoelectron spectrom
19、eters are produced by many manufacturers throughout the world. While the basic principle of the XPS analytical method in each instrument is the same, the specific designs of the instruments and the way that performance specifications are provided differ widely. As a result, it is often difficult to
20、compare the performance of instruments from one manufacturer with those from another. This document provides a basic list of items devised to enable all X-ray photoelectron spectrometers to be described in a common manner. This document is not intended to replace the manufacturers specification, whi
21、ch may extend to 30 or more pages. It is intended that, where certain items are defined in that specification, there is an agreed and defined meaning to that item. ISO 2017 All rights reserved vBS ISO 15470:2017BS ISO 15470:2017Surface chemical analysis X-ray photoelectron spectroscopy Description o
22、f selected instrumental performance parameters1 ScopeThis document describes the way in which specific aspects of the performance of an X-ray photoelectron spectrometer are described.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their con
23、tent constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 18115 (all parts), Surface chemical analysis Vocabulary3 Terms and definitionsFor the pur
24、poses of this document, the terms and definitions given in ISO 18115 (all parts) apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t
25、 t p :/ www .iso .org/ obp4 Abbreviated termsFWHM full width at half maximumXPS X-ray photoelectron spectroscopy5 Description of selected instrumental performance parameters5.1 Method of analysisA short description of the methods used to obtain information from the sample shall be given, and the ava
26、ilability (as an option) of other analytical techniques in the system under consideration shall be stated.5.2 SamplesThe size and shape of samples that may be analysed with the instrument performing to specification shall be given. If the size or shape is restricted for particular modes of analysis,
27、 e.g. angle-resolved measurements, measurements for insulators, etc., this shall be specified.INTERNATIONAL STANDARD ISO 15470:2017(E) ISO 2017 All rights reserved 1BS ISO 15470:2017ISO 15470:2017(E)5.3 System configurationThe designed geometric configuration of significant analytical components of
28、the system and their tolerances shall be described.EXAMPLE Tolerances for angles are often given as 1.5.4 X-ray source5.4.1 Anode typeThe X-ray anode material shall be specified. The energies and relative intensities of unwanted X-rays shall be specified.5.4.2 Anode powerThe maximum X-ray anode powe
29、r shall be specified by stating the potential between the electron source and the X-ray anode and the maximum filament emission current to the anode at that potential. These data shall be given for each of the instrumental operating modes specified, and the analytical areas shall be defined, such as
30、:a) large area;b) defined areas for monochromators;c) high-energy resolution or other relevant modes of operation, as appropriate.5.4.3 Expected anode lifetimeThe expected lifetime of the X-ray anode under the instrumental operating conditions specified in 5.4.2 shall be stated. This is normally a g
31、uaranteed lifetime operation but may, alternatively, be a mean historical lifetime or a graphical description of performance versus operating hours at the instrumental operating modes specified in 5.4.2. The type of lifetime shall be specified.5.5 Spectrometer intensity performance and energy resolu
32、tionThe energy resolution of the system shall be specified by use of the full width at half maximum (FWHM) of the silver Ag 3d5/2peak from a foil of silver cleaned by ion sputtering or scraping such that the intensities of contaminant peaks are less than 5 % of the Ag 3d5/2. Both peak height intensi
33、ty and the FWHM of the Ag 3d5/2peak shall be given for all of the instrumental operating modes specified in 5.4.2. Both the peak height intensity and the FWHM are measured after removal of a straight-line background drawn tangentially at energy points 3 eV above and below the peak position. The ener
34、gy resolution and intensity data may be provided for any other conditions, as required. It is desirable, but not essential, to specify the performance drift over a period of 10 min and 1 h after any required warm-up time.5.6 Spectrometer energy scaleThe repeatability standard deviation of the Cu 2p3
35、/2peak binding energy for samples re-positioned by the positioning procedure shall be given for all sources specified. This procedure should be described in the instrument manual. The binding energy error at the Ag 3d5/2peak position shall be specified when the instrument has been calibrated using t
36、he Cu 2p3/2and the Au 4f7/ 2peaks. The accuracy of the binding energy scale calibration as a function of time shall also be specified at the energy for the Cu 2p3/2or Au 4f7/ 2peaks.NOTE A method for calibrating the binding energy scale of X-ray photoelectron spectrometers is given in ISO 15472.2 IS
37、O 2017 All rights reservedBS ISO 15470:2017ISO 15470:2017(E)5.7 Spectrometer intensity linearityThe maximum useful count rate, and the maximum count rate for a defined limit of count rate linearity, such as 2 %, shall be stated.5.8 Spectrometer response functionEither the spectrometer response funct
38、ion or the energy dependence of that function shall be provided for the relevant instrumental operating modes specified in 5.4.2. The extent to which these functions remain constant with time shall be stated.5.9 Imaging and selected area resolution5.9.1 GeneralImaging systems and selected area syste
39、ms are treated equivalently. The measured value of the lateral resolution shall be obtained by one of the methods described in 5.9.2, 5.9.3 or 5.9.4.5.9.2 Method 1For imaging systems, a sample shall be analysed which has an isolated feature smaller than 30 % of the instruments stated lateral resolut
40、ion. The measured FWHM of a line trace for a photoelectron signal characteristic of that feature defines the lateral resolution. For selected area systems, a sample with a small feature of this kind may be scanned across the analysed area using a micrometer sample stage. The distance for the feature
41、 signal to rise from 50 % of the maximum to 100 % and then fall again to 50 % gives the lateral resolution.NOTE 1 If the width of the isolated feature is greater than 30 % of the lateral resolution, the measured lateral resolution will be greater than the true lateral resolution.NOTE 2 If an instrum
42、ent has a lateral resolution function that can be represented by a Gaussian function, then the FWHM of such a function corresponds to the distance over which the measured signal changes from 12 % to 88 % of its maximum value. The use of a small sample allows easy confirmation of the system astigmati
43、sm.NOTE 3 The lateral resolution may be energy-dependent. A sample of an appropriately sized bulk dot of copper on gold and gold on copper allows the resolution to be specified at both extremes of the energy scale.5.9.3 Method 2For imaging systems, a sample shall be analysed which comprises two mate
44、rials with their surfaces in the same plane and joined along a common straight edge. A line trace for a photoelectron intensity, characteristic of one of the two materials, measured at 90 to the edge, is used to define lateral resolution. For selected area systems, the sample may be scanned across t
45、he analysed area using a micrometer sample stage by movement at 90 to the above edge. For both systems, the distance for the photoelectron intensity to change from 12 % to 88 % of the difference in the intensities in the plateau regions away from the edge defines the lateral resolution in the direct
46、ion of the scan.NOTE 1 If an instrument has a lateral resolution function that can be represented by a Gaussian function, then the FWHM of such a function corresponds to the distance over which the measured signal changes from 12 % to 88 % of its maximum value.NOTE 2 Close to the limit of resolution
47、, astigmatism may be observed, and so the lateral resolution may need determination in more than one azimuth.NOTE 3 Where the analysis area is defined by an electron-optical method using an image aperture, the resolution is defined by the aperture, and the intensity: distance distribution is equival
48、ent to 64 % of the aperture size.NOTE 4 The lateral resolution may be energy-dependent. A sample comprised of copper and gold areas allows the resolution to be specified at both extremes of the energy scale. ISO 2017 All rights reserved 3BS ISO 15470:2017ISO 15470:2017(E)5.9.4 Method 3A sample shall
49、 be analysed which is composed of a knife edge of one material, in the sample plane, over a hole with a depth more than five times its diameter. A line trace for a photoelectron intensity, characteristic of the knife edge material, measured at 90 to the edge, is used to define lateral resolution. The distance for the photoelectron intensity to change from 12 % to 88 % of the difference in the intensities in the plateau regions away from the edge defines the lateral resolution in the direction of the scan.NOTE 1 If an inst
