1、BRITISH STANDARD BS ISO 19318:2004 Surface chemical analysis X-ray photoelectron spectroscopy Reporting of methods used for charge control and charge correction ICS 71.040.40 BS ISO 19318:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 3
2、1 March 2005 BSI 31 March 2005 ISBN 0 580 45709 5 National foreword This British Standard reproduces verbatim ISO 19318:2004 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee CII/60, Surface chemical analysis, which has the re
3、sponsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “Internation
4、al Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British
5、Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and Eu
6、ropean developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 11 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last
7、issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 19318:2004(E) OSI 4002INTERNATIONAL STANDARD ISO 19318 First edition 2004-05-01 Surface chemical analysis X-ray photoelectron spectroscopy Reporting of methods used for charge control and charge correction Analys
8、e chimique des surfaces Spectroscopie de photolectrons Indication des mthodes mises en oeuvre pour le contrle et la correction de la charge BSISO19318:2004IS:81391 O4002(E) DPlcsid Fremia ihTs PDF file may ctnoian emdebt dedyfepcaes. In ccaocnadrw eith Aebods licensilop gnic,y this file mairp eb ynt
9、ed iv roweb detu slahl ton ide ebtlnu deess the typefaces whice era hml era deddebicsnede to i dnanstlaled t noeh computfrep reormign tide ehtin.g In wodlnidaot gnhis file, trapise atpecc tiereht nser ehnopsiiblity fo not infriigngn Aebods licensilop gnic.y ehT ISO tneClar Secrteiraat caceptl on sii
10、bality in this .aera Ai ebods a tredamafo kr Aebod SystemI sncotaropr.de teDails fo teh softwacudorp erts sut deo crtaee this PDF file cna f ebi dnuon tlareneG eh Info leratit evo the file; tP ehDc-Frtaeion marapterew setpo erimizde for irpnti.gn Evyre caer neeb sah taken to sneeru that the file is
11、suitlbae fosu re yb ISO memdob rebeis. In tlnu ehikletneve y ttah lborp aem leratit gno it is f,dnuo plsaee inform ttneC ehlar Secrteiraat ta the serddaig sleb nevwo. ISO 4002 All irthgs erse.devr lnUeto sswrehise specified, on trap fo this lbupictaion maeb y cudorperro de tuilizi den yna form ro na
12、 ybm ynae,s lecetrinoc ro mecinahcal, inclidung tohpcoiypodna gn micrfoilm, wittuoh repmissii non writign from ietI rehSa Ot tsserdda eh ebolw or ISOs memreb i ydobn the cnuotrfo y ttseuqer ehe.r ISO cirypothg fofice saCe tsopale 65 eneG 1121-HC 02 av leT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-
13、mail coirypthgiso.o gr We bwww.is.o gro Pulbisdehi n Switlrez dnaii ISO 4002 Allr ithgsr esedevrBSISO19318:2004IS:81391 O4002(E) I SO 4002 All irthgs ersedevr iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative reference. 1 3 Terms and definitions. 1 4 Symbols and abbreviated terms 1 5
14、 Apparatus. 2 6 Calibration of binding-energy scale 2 7 Reporting of information related to charge control 2 7.1 Methods of charge control. 2 7.2 Information on specimen . 2 7.3 Instrument and operating conditions . 3 7.4 General method for charge control. 3 7.5 Reasons for needing charge control an
15、d for choosing the particular method for charge control 3 7.6 Values of experimental parameters 3 7.7 Information on the effectiveness of the method of charge control . 4 8 Reporting of method(s) used for charge correction and the value of that correction. 4 8.1 Methods of charge correction . 4 8.2
16、Approach 4 8.3 Value of correction energy. 4 Annex A (informative) Description of methods of charge control and charge correction 5 A.1 Introduction. 5 A.2 Methods of charge control. 5 A.3 Methods of charge correction . 7 A.4 Bias referencing17 . 8 A.5 Auger parameter measurements32-34 . 9 Bibliogra
17、phy . 10 BSISO19318:2004IS:81391 O4002(E) iv I SO 4002 All irthgs ersedevrForeword ISO (the International 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 te
18、chnical 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, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates close
19、ly with the International Electrotechnical Commission (IEC) on all matters of electrotechnical 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
20、 International Standards adopted by the technical committees are circulated to the member bodies 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 docume
21、nt may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 19318 was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 5, Auger electron spectroscopy. BSISO19318:2004IS:81391 O4002(E) I SO 4002 All
22、 irthgs ersedevr vIntroduction X-ray photoelectron spectroscopy (XPS) is widely used for characterization of surfaces of materials. Elements in the test specimen (with the exception of hydrogen and helium) are identified from comparisons of the binding energies of their core levels, determined from
23、measured photoelectron spectra, with tabulations of these binding energies for the various elements. Information on the chemical state of the detected elements can frequently be obtained from small variations (typically between 0,1 eV and 10 eV) of the core-level binding energies from the correspond
24、ing values for the pure elements. Reliable determination of chemical shifts often requires that the binding-energy scale of the XPS instrument be calibrated with an uncertainty that could be as small as 0,1 eV. The surface potential of an insulating specimen will generally change during an XPS measu
25、rement due to surface charging, and it is then difficult to determine binding energies with the accuracy needed for elemental identification or chemical-state determination. There are two steps in dealing with this problem. First, experimental steps can be taken to minimize the amount of surface cha
26、rging (charge-control methods). Second, corrections for the effects of surface charging can be made after acquisition of the XPS data (charge- correction methods). Although the buildup of surface charge can complicate analysis in some circumstances, it can be creatively used as a tool to gain inform
27、ation about a specimen. The amount of induced charge near the surface, its distribution across the specimen surface, and its dependence on experimental conditions are determined by many factors including those associated with the specimen and characteristics of the spectrometer. Charge buildup is a
28、well-studied1, 2three-dimensional phenomenon that occurs along the specimen surface and into the material. Charge buildup may also occur at phase boundaries or interface regions within the depth of the specimen that is irradiated by X-rays. Some specimens undergo time-dependent changes in the level
29、of charging because of chemical changes or volatilization induced by photoelectrons and secondary electrons, X-rays, or heating. Such specimens may never achieve steady-state potentials. There is, at present, no universally applicable method or set of methods for charge control or for charge correct
30、ion3, 4 . This International Standard specifies the information that shall be provided to document the method of charge control during data acquisition and/or the method of charge correction during data analysis. Information is given in Annex A on common methods for charge control and charge correct
31、ion that can be useful for many applications. The particular charge-control method that may be chosen in practice depends on the type of specimen (e.g., powder, thin film or thick specimen), the nature of the instrumentation, the size of the specimen, and the extent to which the specimen surface mig
32、ht be modified by a particular procedure. This International Standard is expected to have two main areas of application. First, it identifies information on methods of charge control and/or charge correction to be included in reports of XPS measurements (e.g., from an analyst to a customer or in pub
33、lications) in order to evaluate, assess and reproduce data on insulating materials and to ensure that measurements on similar materials can be meaningfully compared. Second, adherence to this International Standard will enable published binding energies to be used with confidence by other analysts a
34、nd will lead to the inclusion of more reliable data in XPS databases. BSISO19318:2004blank 4002:81391OSISBINTENRATIONAL TSANDADR IS:81391 O4002(E)I SO 4002 All irthgs ersedevr 1Surface chemical analysis X-ray photoelectron spectroscopy Reporting of methods used for charge control and charge correcti
35、on 1 Scope This International Standard specifies the minimum amount of information describing the methods of charge control and charge correction in measurements of core-level binding energies for insulating specimens by X-ray photoelectron spectroscopy that shall be reported with the analytical res
36、ults. Information is also provided on methods that have been found useful for charge control and for charge correction in the measurement of binding energies. 2 Normative reference The following referenced documents are indispensable for the application of this document. For dated references, only t
37、he edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 18115, Surface chemical analysis Vocabulary 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 18115 apply. 4 Symbols
38、 and abbreviated terms BE Binding energy, in eV BE corrCorrected binding energy, in eV BE measMeasured binding energy, in eV BE refReference binding energy, in eV FWHM Full width at half maximum amplitude of a peak in the photoelectron spectrum above the background, in eV XPS X-ray photoelectron spe
39、ctroscopy corrCorrection energy, to be added to measured binding energies for charge correction, in eV BSISO19318:2004IS:81391 O4002(E) 2 I SO 4002 All irthgs ersedevr5 Apparatus 5.1 One or more of the charge-control techniques mentioned in Clause A.2 may be employed in most XPS spectrometers. The X
40、PS instrument shall be operated in accordance with the manufacturers or other documented procedures. 5.2 Some of the techniques outlined in Clause A.2 require special apparatus, such as an electron flood gun or a source for evaporative deposition of gold. 5.3 Certain specimen-mounting procedures, su
41、ch as mounting the specimen under a fine metal mesh5 , can enhance electrical contact of the specimen with the specimen holder, or reduce the amount of surface charge buildup. This and other methods of specimen mounting to reduce static charge are described in detail in ASTM E 1078 and ASTM E 18296,
42、 7 . 6 Calibration of binding-energy scale The binding-energy scale of the X-ray photoelectron spectrometer shall be calibrated using ISO 154728or another documented method before application of this International Standard. 7 Reporting of information related to charge control 7.1 Methods of charge c
43、ontrol Many of the methods commonly used to control the surface potential and to minimize surface charging are summarized in Clause A.2. Information on the following critical specimen and experimental conditions shall be reported for individual specimens or collections of similar specimens. 7.2 Info
44、rmation on specimen 7.2.1 Specimen form The form of the specimen shall be reported. The physical nature, source, preparation method and specimen structure can influence charging behaviour2 . EXAMPLE 1 Powder EXAMPLE 2 Thin film spin-cast on silicon EXAMPLE 3 Macroscopic mineral specimen 7.2.2 Specim
45、en dimensions The size and shape of a specimen can have a significant effect on the extent of specimen charging. The shape of the specimen shall be reported together with approximate values of the dimensions of the specimen or of any relevant specimen features (e.g., particle diameters). 7.2.3 Speci
46、men-mounting methods Specimen mounting and contact with the specimen holder can significantly impact charging1, 2 . The method by which a specimen is mounted, including information about special methods used to increase conductivity or isolate a specimen from ground, shall be reported. EXAMPLE 1 Pow
47、der specimen pressed into foil, which was attached to specimen holder by tape EXAMPLE 2 1 ml of contaminated liquid deposited on a silicon substrate and dried prior to analysis BSISO19318:2004IS:81391 O4002(E) I SO 4002 All irthgs ersedevr 3EXAMPLE 3 Specimen held to holder using conductive adhesive
48、 tape of a specified type EXAMPLE 4 Corroded specimen held on specimen holder by metal screw 7.2.4 Specimen treatment prior to or during analysis The specimen treatment prior to or during analysis includes any physical or chemical treatment that can affect charging of the specimen during XPS measure
49、ments. NOTE Such treatment of the specimen may modify the surface composition as well as the electrical conductivity, and hence charging, of the surface region. 7.3 Instrument and operating conditions The instrument operating conditions include details of the particular XPS instrument, the nature of the X-ray source, the approximate size of the X-ray beam on the specimen surface, the analyser pass energy, a measure of energy resol
