1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 16243:2011Surface chemical analysis Recording and reportingdata in X-ray photoelectronspectroscopy (XPS)BS ISO 16243:2011 BRITISH STANDARDNational forewordThis British Sta
2、ndard is the UK implementation of ISO 16243:2011.The UK participation in its preparation was entrusted to TechnicalCommittee CII/60, Surface chemical analysis.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include
3、 all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 66876 0ICS 71.040.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and
4、Strategy Committee on 31 December 2011.Amendments issued since publicationDate Text affectedBS ISO 16243:2011Surface chemical analysis Recording and reporting data in Xray photoelectron spectroscopy (XPS)Analyse chimique des surfaces Enregistrement et notification des donnes en spectroscopie de phot
5、olectrons par rayons X (XPS) ISO 2011Reference numberISO 16243:2011(E)First edition2011-12-01ISO16243INTERNATIONAL STANDARDBS ISO 16243:2011ISO 16243:2011(E)COPYRIGHT PROTECTED DOCUMENT ISO 2011All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized
6、 in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing 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
7、749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in Switzerlandii ISO 2011 All rights reservedBS ISO 16243:2011ISO 16243:2011(E) ISO 2011 All rights reserved iiiContents PageForeword .vIntroduction .vi1 Scope 12 Normative references .13 Terms and definitions .14 Levels of recording and repor
8、ting 14.1 General .14.2 Analysts record .24.3 Spectra .34.4 Quantitative information 34.5 Compositional depth profiles .44.6 Maps and linescans 44.7 Chemicalstate data 55 Release of data to the customer .5Annex A (informative) Examples of spectra 6Bibliography .9BS ISO 16243:2011ForewordISO (the Int
9、ernational Organization 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 ha
10、s been established has the 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
11、standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies
12、for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.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 a
13、ll such patent rights.ISO 16243 was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 2, General procedures.ISO 16243:2011(E)iv ISO 2011 All rights reservedBS ISO 16243:2011IntroductionX-ray photoelectron spectroscopy (XPS) is used extensively for the surface ana
14、lysis of materials. Elements in the specimen (with the exception of hydrogen and helium) are identified from the measurement of core-level binding energies in the photoelectron spectra, comparing them against elemental tabulations of those energies. Information on the chemical state of such elements
15、 can be derived from the chemical shifts and/or peak shape of the measured photoelectrons with respect to reference states.This International Standard defines the level of information on the specimen and the experimental parameters that should be included in the analytical record. The results of the
16、 analysis should be recorded in a standard format that should include sufficient detail to allow the experiment to be repeated. This material should be available for reporting, as required.Experimental conditions and data acquisition parameters should be included so that the quality of the data can
17、be assessed.ISO 16243:2011(E) ISO 2011 All rights reserved vBS ISO 16243:2011BS ISO 16243:2011INTERNATIONAL STANDARD ISO 16243:2011(E)Surface chemical analysis Recording and reporting data in Xray photoelectron spectroscopy (XPS)1 ScopeThis International Standard specifies the minimum level of infor
18、mation to be reported by the analyst following the analysis of a test specimen using X-ray photoelectron spectroscopy (XPS). It includes information that is to be recorded on or in the analytical record.2 Normative referencesThe following referenced documents are indispensable for the application of
19、 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 18115-1, Surface chemical analysis Vocabulary Part 1: General terms and terms used in spectroscopy3 Terms and definitions
20、For the purposes of this document, the terms and definitions given in ISO 18115-1 and the following apply.3.1ex situoutside the analytical system3.2in situinside the analytical system4 Levels of recording and reporting4.1 GeneralThis International Standard defines the minimum level of information th
21、at shall be recorded and reported by an analyst following the analysis of a test specimen using XPS. The levels of recording and reporting are separated into six main areas:a) the analysts record book or electronic log (e.g. computer data storage system);b) spectra;c) quantitative analysis of the sp
22、ecimen;d) compositional depth profiles;e) maps;f) chemical-shift data. ISO 2011 All rights reserved 1BS ISO 16243:20114.2 Analysts record4.2.1 Specimen identification and preparationFor each individual specimen, the record book or electronic log shall contain the following information (sufficient in
23、formation shall be recorded to allow the measurements to be repeated at a later date):a) the name of the originating laboratory and the person supplying the specimen;b) a unique specimen number;c) a description of the specimen before and after analysis (including details of its physical appearance,
24、its roughness, its colour and any other distinguishing features);d) the date of the measurement(s);e) the name of the analyst, and the analysts department and affiliation;f) all details concerning ex situ specimen preparation before analysis (including the method of mounting, the orientation on the
25、specimen holder with respect to any specific surface features, whether the specimen was cut and, if so, how, details of any solvent cleaning, etc.) (see NOTE 1);g) all details concerning in situ specimen preparation before analysis (including argon ion cleaning, specimen heating, fracture, etc.) (se
26、e NOTE 2).NOTE 1 Guidelines for preparation and mounting of specimens are given in ISO 18116.NOTE 2 Handling of specimens prior to analysis is described in ISO 18117.4.2.2 Analytical conditionsA detailed list of the analytical conditions shall be recorded in the record book and/or the electronic log
27、 (sufficient information shall be recorded to allow the measurements to be repeated at a later date). The information shall include:a) the name or identification of equipment used;b) the X-ray source used and the polarization of the beam, if relevant (Al K, Mg K, monochromated Al K, synchrotron, etc
28、.);c) the X-ray power (record a minimum of two of the following three parameters: power, anode voltage, emission current);d) the analyser input and exit slit widths, if adjustable, and details of any other resolution settings;e) the analyser pass energy (in eV) or retardation ratio;f) the geometry o
29、f irradiation (the direction of the X-ray beam relative to the direction of the detected photoelectron), important for quantitative analysis; the specimen-anode distance in the case of non-monochromated X-ray excitation, if this distance is known.g) the take-off angle used for the measurement;h) the
30、 analysis chamber pressure before and during analysis;i) the area of analysis (as defined by the aperture setting and lens magnification, or as the beam diameter in systems in which the analysis area is determined by the diameter of the X-ray spot);j) the start energy (preferably as a binding energy
31、 or a kinetic energy);k) the end energy or scan width;l) the number of data points, expressed as an integer or as volts/step, and the width of the energy channel;ISO 16243:2011(E)2 ISO 2011 All rights reservedBS ISO 16243:2011m) the acquisition time, expressed as the time/step or as a total time ind
32、icating the measurement time and the X-ray exposure time;n) the charge compensation conditions, if charge compensation is used;o) the value of the acceptance angle for photoelectrons, if this is an instrumental variable;p) when an instrument can be operated in a variety of lens modes, the mode used.
33、All the above information shall be subsequently given to the customer, if requested, along with the analysis of the XPS data by the instrument operator. The customer and the analyst will define the format used to transfer this information. For example, the experimental information may be contained i
34、n the appendix or the experimental section of a report.The binding-energy scale of the X-ray photoelectron spectrometer shall be calibrated either in accordance with ISO 15472 or in accordance with the manufacturers documented calibration procedure.4.3 SpectraAll XPS spectra supplied to a customer s
35、hall include the following minimum information:a) peak or region labels (e.g. C 1s, Cu 2p3/2);b) an abscissa label, e.g. binding energy, EB, or kinetic energy, E;c) abscissa tic marks showing the energy as width of scan, e.g. 0 eV to 1 200 eV, or as energy/division;,d) an ordinate label, showing cou
36、nts, counts/s or simply a scale in arbitrary units;e) ordinate tic marks showing the intensity as counts/s per division or counts per division (counts per channel or counts/s per channel);f) the total acquisition time in the displayed region;g) any energy reference used, such as C 1s (CH) (= 285 eV)
37、 and whether the energy scale has been corrected to this reference;h) details of all the data-processing functions applied to the raw spectrum, for example smoothing, transmission function correction, spike removal.Further information may be included at the discretion of the analyst or at the reques
38、t of the customer. Examples of XPS spectra are shown in Annex A (see Figures A.1 and A.2).4.4 Quantitative informationWhen the XPS data are processed and supplied to a customer as quantitative data, the following information on the method of quantification shall also be made available to the custome
39、r, if required:a) the quantification model, e.g. homogeneous solid, homogeneous solid under a contamination layer, layered solid;b) the name and version of the data-processing software used;c) the type of background fitted to the data, with start and end points, if appropriate;d) the sensitivity fac
40、tors used (including whether by height or by area) and their source, e.g. manufacturers, in-house standards, theory;e) any other correction terms used and their justification, e.g. specimen roughness, backscattering, matrix effects;f) the estimated error, as discussed for example in ISO 20903;ISO 16
41、243:2011(E) ISO 2011 All rights reserved 3BS ISO 16243:2011g) when the atomic fraction of components having particular chemical states are reported, the method used to separate the peak height or peak area from adjacent peaks;h) if curve fitting (peak synthesis) was used, the function(s) used (e.g.
42、Gaussian), any constraints, and a measure of the goodness of fit;i) details of any corrections made for deadtime, spectrometer window, etc.;j) details of any elements specifically excluded from the quantification procedure (such as carbon surface contaminant).4.5 Compositional depth profilesComposit
43、ional depth profiles may be presented as a montage of spectra or as depth profiles derived from peak area or peak height measurements on spectra. If the data are quantified, the factors listed in 4.4 shall be considered, and noted where appropriate. In addition, the depth of analysis of ion-sputtere
44、d depth profiles may be estimated with respect to the sputter rate of a standard material under the same conditions (see Figure A.3 in Annex A).NOTE The measurement of sputtered depth in depth profiling is described in ISO/TR 15969.Where depth profiles are acquired from taper sections or dimpled cra
45、ters, the depth can be estimated by geometrical calculation.The following information shall be available to be supplied with the compositional depth profiles, if required:a) an ordinate label, e.g. atomic fraction (together with details of quantification as outlined in 4.4), or nominal counts;b) ord
46、inate tic marks showing the atomic fraction, counts/s, counts or simply a scale in arbitrary units);c) an abscissa label, i.e. sputtering time or estimated depth;d) abscissa tic marks showing time or depth;e) for ion-sputtered profiles, the sputtering rate and the sputtering-rate calibration materia
47、l used;f) details of the ion beam energy and diameter, the ion beam current and the area sputtered or rastered.4.6 Maps and linescansWhen XPS maps or linescans (see Annex A, Figure A.4) are provided, the following information shall be supplied to the customer, as required (if the information is prov
48、ided as part of a depth profile, also include the details requested in 4.5):a) the identity of XPS peak and/or area that has been mapped, together with details of any background removal procedure;b) details of the map field of view (X and Y directions);c) details of the map field of view calibration
49、 in the X and Y directions;d) details of the property mapped, e.g. atomic percentage, together with a scale indicating the colour, if appropriate;e) the method used to obtain the map, e.g. parallel acquisition, stage scanning, X-ray beam scanning, input lens scanning.ISO 16243:2011(E)4 ISO 2011 All rights reservedBS ISO 16243:20114.7 Chemicalstate dataIf the XPS spectra are analysed for chemical-state information, the following experimental information shall be attached to the collection of spectra:a) the element and the chemical f
