1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 10810:2010Surface chemical analysis X-ray photoelectron spectroscopy Guidelines for analysisBS ISO 10810:2010 BRITISH STANDARDNational forewordThis British Standard is the
2、 UK implementation of ISO 10810:2010.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 all the nec
3、essaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 65043 7ICS 71.040.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Com
4、mittee on 31 December 2010.Amendments issued since publicationDate Text affectedBS ISO 10810:2010Reference numberISO 10810:2010(E)ISO 2010INTERNATIONAL STANDARD ISO10810First edition2010-11-15Surface chemical analysis X-ray photoelectron spectroscopy Guidelines for analysis Analyse chimique des surf
5、aces Spectroscopie de photolectrons par rayons X Lignes directrices pour lanalyse BS ISO 10810:2010ISO 10810:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typeface
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10、.iso.org Published in Switzerland ii ISO 2010 All rights reservedBS ISO 10810:2010ISO 10810:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Symbols and abbreviations1 5 Overview of sample analysis .2 6 Spe
11、cimen characterization.4 6.1 General .4 6.2 Specimen forms.4 6.3 Material types.6 6.4 Handling and mounting of specimens 7 6.5 Specimen treatments 7 7 Instrument characterization87 7.1 General .7 7.2 Instrument checks.8 7.3 Instrument calibration.8 7.4 Instrument set-up 14 8 The wide-scan spectrum.1
12、5 8.1 Data acquisition.15 8.2 Data analysis16 9 The narrow scan18 9.1 General .18 9.2 Data acquisition.18 9.3 Data analysis18 10 Test report22 Bibliography24 BS ISO 10810:2010ISO 10810:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a world
13、wide 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 the right to be represented on t
14、hat 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. International Standards are drafted in
15、 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 for voting. Publication as an International Standard
16、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 all such patent rights. ISO 10810 was prepared by Tec
17、hnical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 7, X-ray photoelectron spectroscopy. BS ISO 10810:2010ISO 10810:2010(E) ISO 2010 All rights reserved vIntroduction X-ray photoelectron spectroscopy (XPS) is used extensively for the surface analysis of materials. Elements in the
18、 sample (with the exception of hydrogen and helium) are identified from comparisons of the measured binding energies of their core levels with tabulations of those energies for the different elements. Their chemical states may be determined from shifts in peak positions and other parameters compared
19、 with the data for that element in its pure elemental state. Information on the quantities of such elements can be derived from the measured intensities of photoelectron peaks. Calculation of the quantities of the constituent chemical species present in the surface layer studied may then be made usi
20、ng formulae and relative-sensitivity factors provided by the spectrometer manufacturer or locally measured relative-sensitivity factors and appropriate software. This guidance document is intended to aid the operator of X-ray photoelectron spectrometers to obtain efficient, meaningful analyses from
21、typical samples. BS ISO 10810:2010BS ISO 10810:2010INTERNATIONAL STANDARD ISO 10810:2010(E) ISO 2010 All rights reserved 1Surface chemical analysis X-ray photoelectron spectroscopy Guidelines for analysis 1 Scope This International Standard is intended to aid the operators of X-ray photoelectron spe
22、ctrometers in their analysis of typical samples. It takes the operator through the analysis from the handling of the sample and the calibration and setting-up of the spectrometer to the acquisition of wide and narrow scans and also gives advice on quantification and on preparation of the final repor
23、t. 2 Normative references The following referenced documents are indispensible for the application of this document. For dated references only the cited edition applies. For undated references, the latest edition of the referenced document (together with any amendments) applies. ISO/IEC 17025, Gener
24、al requirements for the competence of testing and calibration laboratories ISO 18115-1, Surface chemical analysis Vocabulary Part 1: General terms and terms used in spectroscopy 3 Terms and definitions For the purposes of this International Standard, the terms and definitions given in ISO 18115-1 ap
25、ply. 4 Symbols and abbreviations AES Auger electron spectroscopy ARXPS angle-resolved X-ray photoelectron spectroscopy CCQM consultative committee for amount of substance CRM certified reference material EAL effective attenuation length FAT fixed analyser transmission FRR fixed retard ratio FWHM ful
26、l width at half maximum IERF intensity/energy response function NIST National Institute of Standards and Technology NPL National Physical Laboratory RM reference material RSD residual standard deviation S/N signal-to-noise ratio BS ISO 10810:2010ISO 10810:2010(E) 2 ISO 2010 All rights reservedXPS X-
27、ray photoelectron spectroscopy 1difference between the measured and reference energies for Au 4f7/24difference between the measured and reference energies for Cu 2p3/25 Overview of sample analysis Figure 1 is a flow chart illustrating the analysis of a typical sample by XPS. A preliminary consultati
28、on with the supplier of the sample should be used to ensure that the sample is supplied in the form most appropriate for analysis. ISO 181172explains the issues involved with prior handling by the supplier and also gives information on the most suitable container for transportation. In this consider
29、ation, the analyst should also identify any particular problems likely to arise. Table 1 provides a list of example problems. Prior to any work, discussions should be held between the analyst and the customer to gain as much information as possible by reviewing what is already known regarding the sa
30、mple and its history. In addition to the information listed in ISO 181172, Table 2 indicates information that will assist in deciding how to conduct the XPS analysis. Following these preliminary discussions, the sample(s) may need to be prepared to allow mounting in the spectrometer and to reduce, w
31、here possible, the subsequent analysis time. ISO 181161provides details of how to do this. The analyst will be responsible for the instrument characterization, which will include the calibration state and the overall performance of the XPS instrument. A guide to calibration of the energy scale is gi
32、ven in ISO 1547214. Checks for the intensity scale are given in ISO 242379and ISO 2127018. Once the specimen has been mounted in the spectrometer and the system pumped down, data acquisition can commence. A wide scan should be obtained first and this then analysed to determine the elements present.
33、ISO 1624331provides information on recording and reporting data in XPS. The wide-scan spectrum can provide qualitative and semi-quantitative information regarding composition and the depth distribution of species. This may yield sufficient information to satisfy the customer and the analysis may be
34、terminated. However, in most cases, more data are required and narrow-scan spectra will then be recorded from regions identified in the wide-scan spectrum. Analysis of these narrow-scan spectra will provide chemical-state information, more accurate quantitative information and near-surface depth inf
35、ormation. At a later time in the investigation the wide scan should be repeated to determine if there has been degradation (e.g. due to X-ray irradiation or to surface reactions with ambient gases in the vacuum system). Following evaluation of the XPS data, the analyst should produce a report. Table
36、 1 Problems likely to arise and related ISO standards Problem Example ISO Standard Outgassing Water vapour ISO 18116 Degradation Polymers and organics Charging Insulators ISO 1931828Reduction Oxides Contaminant mobility Chlorine Sample containment Powders ISO 18116 Surface topography Fibres Table 2
37、Sample information and history Sample information and history Thermal Contamination Possible composition Segregation Surface layer Homogeneous Islands BS ISO 10810:2010ISO 10810:2010(E) ISO 2010 All rights reserved 3Figure 1 Flow chart of an XPS analysis (The numbers in brackets indicate the respect
38、ive subclauses in this International Standard.) BS ISO 10810:2010ISO 10810:2010(E) 4 ISO 2010 All rights reserved6 Specimen characterization 6.1 General The complexity of the interacting factors in XPS analyses arises from the many different forms of specimen materials and the variety of material ty
39、pes that may be encountered as well as from the different XPS experiments that might be required. Table 3 illustrates possible specimen forms, material types, and XPS experiments or issues for further review. The analyst should also be aware that samples can consist of multiple components and phases
40、, and that identification of the components and phases present (and their spatial arrangements) can be an important part of an XPS analysis. A further complication is that non-conducting samples may charge. Table 3 Some specimen forms, material types, in situ specimen treatments and possible XPS exp
41、eriments Specimen forms Material types In situ specimen treatments XPS experiments Adsorbed layers (6.2.3) Alloy (6.3.2) Cooling (6.5.2) Angle-resolved XPS Amorphous Biological (6.3.9) Degradation Analysis area (small) Fibres (6.2.8) Catalyst (6.3.7) Deposit thin films Analysis area (large) Films (6
42、.2.3) Ceramic (6.3.6) Expose to high gas pressure (6.5.5) Depth profile Interface (6.2.4) Composite Fracture (6.5.3) Imaging Internal interface (6.2.9) Glass (6.3.8) Heating (6.5.2) Line scan Liquid Insulator (6.3.8) Insert into liquids (6.5.5) Multilayered (6.2.4) Magnetic metal (6.3.5) Ion bombard
43、ment (6.5.4) Nano-material Metal (6.3.2) Scraping (6.5.3) Non-porous (6.2.5) Non-metal (pure) element Pattern system Polymer (6.3.3) Polycrystal Semiconductor (6.3.4) Porous (6.2.6) Textile Powder (6.2.7) Residue (6.2.3) Segregated layer (6.2.3) Single crystal (6.2.2) Solid Textile (6.2.8) Contamina
44、tion 6.2 Specimen forms 6.2.1 General The form of the specimen to be analysed will strongly dictate the kinds of experimental approach that can and need to be employed. BS ISO 10810:2010ISO 10810:2010(E) ISO 2010 All rights reserved 56.2.2 Single crystal This type of sample should have a flat surfac
45、e. Quantitative analyses will generally be difficult because of anisotropies in the angular distributions of the photoemitted electrons due to electron diffraction or to forward-focussing effects34. These anisotropies are nevertheless useful in determining the structural properties of the sample. 6.
46、2.3 Adsorbed or segregated layers, films and residues It should, in general, be possible to obtain a quantitative analysis and chemical-state information for adsorbed or segregated layers, films and residues56. If the substrate is a single crystal, however, quantitative analyses will generally be di
47、fficult, but the angular distributions of the photoemitted electrons can give useful structural information3. Angle-resolved XPS (ARXPS), as described in 9.3.3, will enable the layer thickness to be determined, provided the layer thickness does not exceed around three times the effective attenuation
48、 length (EAL) of the substrate peak. This will be of progressively lower accuracy for films above one EAL in thickness. 6.2.4 Interfaces and multilayered samples Ion sputter depth profiling should permit the depth distribution and thickness of the layers to be determined, together with a semi-quanti
49、tative analysis of the layers, as described in 9.3.3. 6.2.5 Non-porous A quantitative analysis together with chemical-state information can be obtained. 6.2.6 Porous Only a semi-quantitative analysis may be possible since the sample will have a rough surface. 6.2.7 Powder Mount the sample by embedding in a suitable matrix. In many cases, indium proves sufficiently soft to be able to accept the powder without particles falling off. Then treat the composite sample as a porous sample
