1、Designation: E2735 13Standard Guide forSelection of Calibrations Needed for X-ray PhotoelectronSpectroscopy (XPS) Experiments1This standard is issued under the fixed designation E2735; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This guide describes an approach to enable users andanalysts to determine the calibrations and standards
3、 useful toobtain meaningful surface chemistry data with X-ray photo-electron spectroscopy (XPS) and to optimize the instrument forspecific analysis objectives and data collection time.1.2 This guide offers an organized collection of informationor a series of options and does not recommend a specific
4、 courseof action. This guide cannot replace education or experienceand should be used in conjunction with professional judgment.Not all aspects of this guide will be applicable in all circum-stances.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are in
5、cluded in thisstandard.1.4 This standard is not intended to represent or replace thestandard of care by which the adequacy of a given professionalservice must be judged, nor should this document be appliedwithout consideration of a projects many unique aspects. Theword “Standard” in the title of thi
6、s document means only thatthe document has been approved through the ASTM consensusprocess.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practi
7、ces and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E684 Practice for Approximate Determination of CurrentDensity of Large-Diameter Ion Beams for Sputter DepthProfiling of Solid Surfaces (Withdrawn 2012)3E995 Guide for Background Sub
8、traction Techniques in Au-ger Electron Spectroscopy and X-Ray PhotoelectronSpectroscopyE996 Practice for Reporting Data in Auger Electron Spec-troscopy and X-ray Photoelectron SpectroscopyE1016 Guide for Literature Describing Properties of Elec-trostatic Electron SpectrometersE1078 Guide for Specime
9、n Preparation and Mounting inSurface AnalysisE1127 Guide for Depth Profiling in Auger Electron Spec-troscopyE1217 Practice for Determination of the Specimen AreaContributing to the Detected Signal in Auger ElectronSpectrometers and Some X-Ray Photoelectron Spectrom-etersE1523 Guide to Charge Control
10、 and Charge ReferencingTechniques in X-Ray Photoelectron SpectroscopyE1577 Guide for Reporting of Ion Beam Parameters Used inSurface AnalysisE1634 Guide for Performing Sputter Crater Depth Measure-mentsE1636 Practice for Analytically Describing Depth-Profileand Linescan-Profile Data by an Extended L
11、ogistic Func-tionE1829 Guide for Handling Specimens Prior to SurfaceAnalysisE2108 Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer2.2 ISO Standards:4ISO 10810 Surface Chemical AnalysisDepth ProfilingMeasurement of Sputtered DepthISO 14606 Surface C
12、hemical AnalysisSputter DepthProfilingOptimisation Using Layered Systems as Ref-erence MaterialsISO 14701 Surface Chemical AnalysisX-ray Photoelec-tron SpectroscopyMeasurement of Silicon Oxide Thick-ness1This guide is under the jurisdiction of ASTM Committee E42 on SurfaceAnalysis and is the direct
13、responsibility of Subcommittee E42.03 on Auger ElectronSpectroscopy and X-Ray Photoelectron Spectroscopy.Current edition approved Jan. 15, 2013. Published January 2013. DOI: 10.1520/E2735-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serv
14、iceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor
15、, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1ISO 14976 Surface Chemical AnalysisData Transfer For-matISO 15470 Surface Chemical AnalysisX-ray Photoelec-tron SpectroscopyDescription of Select
16、ed InstrumentalPerformance ParametersISO 15472 Surface Chemical AnalysisX-ray Photoelec-tron SpectrometersCalibration of Energy ScalesISO/TR 15969 Surface Chemical AnalysisDepthProfilingMeasurement of Sputtered DepthISO 18115-1 Surface Chemical AnalysisVocabularyPart 1: General Terms and Terms Used
17、in SpectroscopyISO 18115-2 Surface Chemical AnalysisVocabularyPart 2: Terms Used in Scanning-ProbeISO 18116 Surface Chemical AnalysisGuidelines forPreparation and Mounting of Specimens for AnalysisISO 18117 Surface Chemical AnalysisHandling of Speci-mens Prior to AnalysisISO 18118 Surface Chemical A
18、nalysisAuger ElectronSpectroscopy and X-ray Photoelectron SpectroscopyGuide to the Use of Experimentally Determined RelativeSensitivity Factors for the Quantitative Analysis of Ho-mogeneous MaterialsISO/TR 18392 Surface Chemical AnalysisX-ray Photo-electron SpectroscopyProcedures for DeterminingBack
19、groundsISO 18516 Surface Chemical AnalysisAuger ElectronSpectroscopy and X-ray Photoelectron SpectroscopyDetermination of Lateral ResolutionISO 19318 Surface Chemical AnalysisX-ray Photoelec-tron SpectroscopyReporting of Methods Used forCharge Control and Charge CorrectionISO/TR 19319 Surface Chemic
20、al AnalysisAuger ElectronSpectroscopy and X-ray Photoelectron SpectroscopyDetermination of Lateral Resolution, Analysis Area andSample Area Viewed by the AnalyserISO 20903 Surface Chemical AnalysisAuger ElectronSpectroscopy and X-ray Photoelectron SpectroscopyMethods Used to Determine Peak Intensiti
21、es and Infor-mation Required when Reporting ResultsISO 21270 Surface Chemical AnalysisX-ray Photoelec-tron and Auger Electron SpectrometersLinearity ofIntensity ScaleISO 22335 Surface Chemical AnalysisDepth ProfilingMeasurement of Sputtering Rate: Mesh-Replica MethodUsing a Mechanical Stylus Profilo
22、meterISO 24237 Surface Chemical AnalysisX-ray Photoelec-tron SpectroscopyRepeatability and Constancy of In-tensity Scale3. Terminology3.1 DefinitionsFor definitions of surface analysis termsused in this guide, see ISO 18115-1 and ISO 18115-2.4. Significance and Use4.1 The purpose of this guide is as
23、sist users and analysts inselecting the standardization procedures relevant to a definedXPS experiment. These experiments may be based, forexample, upon material failure analysis, the determination ofsurface chemistry of a solid, or the composition profile of a thinfilm or coating. A series of optio
24、ns will be summarized givingthe standards that are related to specific information require-ments. ISO 15470 and ISO 10810 also aid XPS users inexperiment design for typical samples. ASTM Committee E42and ISO TC201 are in a continuous process of updating andadding standards and guides. It is recommen
25、ded to refer to theASTM and ISO websites for a current list of standards.5. Procedure5.1 General Sample Characterization:5.1.1 Sample HistoryThe analyst should obtain a sum-mary of the background information of the sample, includingdescriptors, history, sample cleaning and handling, existingapplicat
26、ion data, bulk composition, and any prior analysis thathas been conducted. The sample history, especially handling,packing and storage, can impact the approach needed to obtainthe desired information. Because inadequate sample collectioncan sometimes destroy or minimize the ability to collect thedes
27、ired information, it is often necessary to identify the neededinformation and establish the procedures to be used (5.2)before the surface analysis is performed.5.1.2 Vacuum CompatibilityThe compatibility of samplewith instrument vacuum should be considered. Although somesamples have inappropriately
28、high vapor pressures for ambienttemperature operation, some instruments may include a samplecooling stage, which allows these types of materials to beanalyzed. Additionally, newer XPS systems often have im-proved vacuum pumps coupled with monochromatic X-raysources (that do not heat the sample) and
29、a small X-ray spotsize (requiring less sample for analysis). As a result, stronglyoutgassing or subliming samples can often be examined.5.2 Design of Experiment:5.2.1 The goal of the experiment should be defined. Experi-mental goals may include data relating to the surface chemicalcomposition and ch
30、emical state, surface segregation,quantification, layer thickness, nanostructures, and so forth.The identification of the specific analysis objectives influencessample handling, instrument setup, the approach to datacollection, and finally the methods of data analysis.5.2.1.1 Table 1 is a summary of
31、 possible experiments alongwith different calibrations to be considered.5Also included arethe ASTM and ISO standards for checking the parameter. Inthe table, an X indicates applications where a calibration isrequired. Additionally, the calibrations are ranked with X =generally important and XX = gen
32、erally very important cali-brations for a given task.5.2.2 General System CheckThe analyst should perform ageneral system health check (including mechanicalcomponents, sample holders, vacuum level, and performancecheck) as recommended by the instrument manufacturer. Manyanalysts have also developed
33、their own methods to verify thegeneral operational health of an instrument. This might bedone, for example, by testing a specimen commonly analyzedby the instrument to quickly verify the binding energies of few5Castle, J. E., Powell, C. J., Report on the 34th IUVSTA Workshop, XPS: FromSpectra to Res
34、ultsTowards an Expert System, Surface and Interface Analysis,Vol26, 2004, pp. 225237.E2735 132photoelectron peaks and overall count rates. Based upon theexperiment to be performed, the relative importance of theparameters in Table 1 should be assessed, including calibrationof the binding-energy scal
35、e, intensity repeatability andconstancy, intensity/energy response function (IERF), linearitytest of the intensity scale, energy resolution for the desiredintensity, lateral resolution, charge compensation, depthresolution, and depth profile rate calibration.5.2.3 Sample Transport and PreparationAs
36、a surfaceanalysis technique, X-ray photoelectron spectroscopy (XPS) issensitive to the outermost few atomic layers of the samplebeing characterized. Specimens should be transported to theanalyst in a container that does not come into direct contactwith the surface of interest. In most cases, the ana
37、lysis will beperformed on the as-received specimen; therefore, the goalmust be to preserve the state of the surface so that the analysisremains representative of the original surface. Care must thenbe taken to ensure that no outside agents come in contact withthe surface to be investigated. These ag
38、ents include: fingers,solvents or cleaning solutions, gases (including compressedair) or vapors, metals, tissue or other wrapping materials, tape,cloth, tools, packing materials or the walls of containers.Handling of the surface to be analyzed should be eliminated orminimized whenever possible.5.2.3
39、.1 Proper preparation and mounting of specimens isparticularly critical for surface analysis. Improper preparationof specimens can result in alteration of the surface compositionand unreliable data. In addition, specimen mounting techniqueshave the potential to affect the intended analysis.Guides E1
40、078 and E1829 and/or ISO 18116 and ISO 18117TABLE 1 Recommended XPS Calibrations for Defined ExperimentsNOTE 1Calibrations required to obtain meaningful data or to optimize the instrument for the best data in the time available.AThe X indicatesapplications where a calibration is required. X = genera
41、lly important, XX = generally very important. Local methods are procedures developed by anindividual laboratory or the instrument manufacturer. NPL software for the calibration of the intensity scales of XPS instruments is available from theUK National Physical Laboratory.BBCR 261Cis a certified ref
42、erence tantalum oxide/tantalum foil calibration sample and NIST SRM 2135cDis a certifiednickel/chromium thin-film depth profile standard.InstrumentCalibrationsand ChecksASTMStandardISOStandardElementalCompositionChemicalStateLow LevelDetectionQuantifi-cationLayerThicknessNano-structuresGeneral Syste
43、m Check Local Method Local Method XX XX XX XX XX XXSample Preparation E1829E10781811618117XXXXBinding Energy E2108E15231547219318XX XX X XIntensity Repeatabilityand Constancy24237 X X XX XX X XIntensity/Energy Re-sponse FunctionNPLSoftwareXX X XXLinearity of IntensityScaleE1016 2127018118XX XXXPeak
44、Intensities E995,Local Method1839220903XXXXXXIon Gun and SputterRateE684E1577E1127E16341596922335BCR 2611460614701XX XXDepth Resolution E684E1577E1127E1634E1636BCR 261NIST SRM2135c14606XX XXAnalysis Area E1217 19319 X X X XXLateral Resolution 18516 X X X XData Reporting E996 14979 X X X X X XACastle
45、, J. E., Powell, C. J., Report on the 34th IUVSTA Workshop, XPS: From Spectra to ResultsTowards an Expert System, Surface and Interface Analysis, Vol 26,2004, pp. 225237.BNational Physical Laboratory (NPL), http:/www.npl.co.uk/server.php?show=ConWebDoc.606.CEuropean Institute for Reference Materials
46、 and Measurements, BCR261, certified reference material.DNational Institute of Standards and Technology, NIST-SRM 3125c Ni/Cr Thin Film Depth Profile Standard, http:/www.nist.gov/srm.E2735 133describe methods the surface analyst may need to minimize theeffects of specimen preparation when using any
47、surface-sensitive analytical technique. Also described are methods tomount specimens so as to ensure that the desired information isnot compromised. Because of the wide range of types ofspecimens and desired information, only broad guidelines andgeneral examples are included in the standards. The op
48、timumhandling procedures will be dependent on the particularspecimen and the needed information. It is recommended thatthe specimen supplier consult the surface analyst as soon aspossible with regard to specimen history, the specific problemto be solved or information needed, and the particular spec
49、i-men preparation or handling procedures required.5.2.4 Binding Energy, Energy Scale Linearity, and ChargeCompensationCalibrations of the binding energy (BE) scalesof XPS instruments are required for four principal reasons.First, meaningful comparison of BE measurements from two ormore XPS instruments requires that the BE scales becalibrated, often with an uncertainty of about 0.1 to 0.2 eV.Second, identification of chemical state is based on measure-ment of chemical shifts of photoelectron and Auger-electronfeatures, again with an
