1、Designation: E1016 07 (Reapproved 2012)1Standard Guide forLiterature Describing Properties of Electrostatic ElectronSpectrometers1This standard is issued under the fixed designation E1016; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, 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.1NOTEEditorial corrections were made throughout in November 2012.1. Scope1.1 The purpose of this guide is to fam
3、iliarize the analystwith some of the relevant literature describing the physicalproperties of modern electrostatic electron spectrometers.1.2 This guide is intended to apply to electron spectrometersgenerally used in Auger electron spectroscopy (AES) andX-ray photoelectron spectroscopy (XPS).1.3 The
4、 values stated in inch-pound units are to be regardedas standard. No other units of measurement are included in thisstandard.1.4 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 app
5、ro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E673 Terminology Relating to Surface Analysis (Withdrawn2012)3E902 Practice for Checking the Operating Characteristics ofX-Ray Photoelectron Spectr
6、ometers (Withdrawn 2011)3E1217 Practice for Determination of the Specimen AreaContributing to the Detected Signal in Auger ElectronSpectrometers and Some X-Ray Photoelectron Spectrom-etersE2108 Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer2.2 IS
7、O Standards:4ISO 18516 Surface Chemical AnalysisAuger ElectronSpectroscopy and X-Ray Photoelectron SpectrsocopyDetermination of Lateral ResolutionISO 21270 Surface Chemical AnalysisX-Ray Photoelec-tron and Auger Electron SpectrometersLinearity ofIntensity ScaleISO 24236 Surface Chemical AnalysisAuge
8、r ElectronSpectroscopyRepeatability and Constancy of IntensityScaleISO 24237 Surface Chemical AnalysisX-Ray Photoelec-tron SpectroscopyRepeatability and Constancy of In-tensity Scale3. Terminology3.1 For definitions of terms used in this guide, refer toTerminology E673.4. Summary of Guide4.1 This gu
9、ide serves as a resource for relevant literaturewhich describes the properties of electron spectrometers com-monly used in surface analysis.5. Significance and Use5.1 The analyst may use this document to obtain informa-tion on the properties of electron spectrometers and instrumen-tal aspects associ
10、ated with quantitative surface analysis.6. General Description of Electron Spectrometers6.1 An electron spectrometer is typically used to measurethe energy and angular distributions of electrons emitted froma specimen, typically for energies in the range 0 to 2500 eV. Insurface analysis applications
11、, the analyzed electrons are pro-duced from the bombardment of a sample surface withelectrons, photons or ions. The entire spectrometer instrumentmay include one or more of the following: (1) apertures todefine the specimen area and emission solid angle for the1This guide is under the jurisdiction o
12、f ASTM Committee E42 on SurfaceAnalysis and is the direct responsibility of Subcommittee E42.03 on Auger ElectronSpectroscopy and X-Ray Photoelectron Spectroscopy.Current edition approved Nov. 1, 2012. Published December 2012. Originallyapproved in 1984. Last previous edition approved in 2007 as E10
13、16 07. DOI:10.1520/E1016-07R12E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version
14、of this historical standard is referenced onwww.astm.org.4Available from International Organization for Standardization (ISO), 1 rue deVaremb, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19
15、428-2959. United States1electrons accepted for analysis; (2) an electrostatic or magneticlens system, or both; (3) an electrostatic (dispersing) analyzer;and (4) a detector. Methods to check the operating character-istics of X-ray photoelectron spectrometers are reported inPractice E902.6.2 Intensit
16、y Scale Calibration and Spectrometer Transmis-sion FunctionQuantitative analysis requires the determina-tion of the ability of the spectrometer to transmit electrons, andthe resultant detector signal, throughout the spectrometerinstrument. This can be described by an overall electronenergy-dependent
17、 transmission function Q(E) and is given bythe product (1, 2),5as follows:QE! 5 HE!TE!DE!FE!, (1)where:H(E) = the effect of mechanical imperfections (such asaberrations, fringing fields, etc.),T(E) = electron-optical transmission function,D(E) = detector efficiency, andF(E) = efficiency of the count
18、ing systems.Knowledge of this transmission function permits the cali-bration of the spectra intensity axis (3).Adetailed review of theexperimental determination of the transmission function forXPS (4) and AES (5) measurements has been published.6.3 Energy Scale CalibrationCalibration of the energysc
19、ales of AES and XPS instruments is required for (1)meaningful comparison of building-energy or kinetic-energymeasurements from two or more instruments; (2) valid identi-fication of chemical state from such comparisons; (3) effectiveuse of databases containing reported energy values; and (4)asa compo
20、nent of a laboratory quality system. Suitable photonenergy values forAl and Mg anode X-ray sources often used inXPS measurements are available (6) and reference bindingenergy values for copper (Cu), gold (Au), and silver (Ag) havebeen published (7). Reference kinetic-energy values for Cu,aluminium (
21、Al), and Au are also available (8, 9). Bindingenergy scale calibration procedures have been described in theliterature for XPS (10, 11) and kinetic energy scale calibrationsfor AES (8, 12-14) measurements. Practice E2108 describes aprocedure for calibrating the binding energy scale of XPSinstruments
22、 using Cu, Ag, and Au specimens.6.4 Linearity of Intensity ScaleSee ISO 21270 for meth-ods to evaluate linearity of the intensity scale of AES and XPSspectrometers.6.5 Repeatability and Constancy of Intensity ScaleSeeISO 24236 and ISO 24237 for methods to evaluate the repeat-ability and constancy of
23、 intensity scales of AES and XPsspectrometers, respectively.6.6 Lateral ResolutionSee ISO 18516 for methods todetermine the lateral resolution of AES and XPS spectrom-eters.6.7 Specimen Area Contributing to the Detect SignalSeePractice E1217 for methods to determine the specimen areacontributing to
24、the detected signal in Auger electron spectrom-eters and some X-Ray photoelectron spectrometers.6.8 Calibration ProtocolRecommendations have beenpublished describing spectrometer calibration requirementsand the frequency with which AES and XPS spectrometersshould be calibrated (15).7. Literature7.1
25、Electrostatic AnalyzersSpectrometers commonly usedon modern AES and XPS spectrometer instruments generallyemploy electrostatic deflection analyzers. Auger electron spec-trometers often use cylindrical mirror analyzer (CMA) designs,although concentric hemispherical analyzers (CHA) (alsoknown as spher
26、ical deflection (or sector) analyzers) are alsoused. The CHA design is the most common analyzer employedon modern XPS instruments, although double-pass CMAdesigns were also employed on earlier XPS instruments.Retarding field analyzers (RFA) have historical interest in earlyAES work, but are now comm
27、only used on low energy electrondiffraction apparatus.7.1.1 Electrostatic Deflection Analyzers A review of thegeneral properties of deflection analyzers may be found inreview articles (16, 17). More detailed reviews are alsoavailable where, in addition to the CMA and CHA designs,plane mirror, spheri
28、cal mirror, cylindrical sector, and toroidaldeflection analyzers are treated (18-20).As the width of typicalAuger spectral features are several electron volts, the use of aCMA design in conventional AES has sufficed for routineanalysis, particularly for small area analysis where a compro-mise betwee
29、n signal-to-noise and energy resolution is impor-tant. These are commonly used at a resolution defined by thefull-width at half-maximum of the spectrometer energyresolution, E, divided by the electron energy, E, of 0.25 to0.6 %. The ability to incorporate an electron source concentricwith the CMAaxi
30、s has been extensively exploited in scanning-electron microscope instruments to give Auger data as afunction of beam position (that is, images). However, analysisof the Auger spectra from some compounds and surfacemorphologies may be enhanced by the use of a CHA designwhich can provide better energy
31、 resolution (but a lowertransmission) and superior angular resolution. The CHAdesignis most frequently employed on XPS instruments wherespectral features generally have narrow energy widths of 1 eVor less and higher angular resolution is desired for the detectedelectrons than is possible with a CMA.
32、 The relationshipbetween the pass energy of various spectrometer designs andthe potential between their electrodes is described in detail(16).7.1.2 Retarding Field AnalyzersThe use of a retardingfield analyzer (RFA), consisting of concentric, spherical-sectorgrids, is currently used most commonly on
33、 electron diffractioninstruments where the angular distribution of the detectedelectrons is examined. See also a brief review of RFA designs(16) and a substantial report on resolution and sensitivity issues(21).7.2 AperturesThe effects of the spectrometer entrance andexit slits and apertures, their
34、associated fringing fields, as well5The boldface numbers in parentheses refer to the list of references at the end ofthis guide.E1016 07 (2012)12as the effect of the divergence of the incident electron trajec-tories on analyzer performance, particularly energy resolution,have also been reviewed (16-
35、20).Adetailed examination of theeffects of unwanted internal scattering in CHA and CMAelectron spectrometers has been reported in the literature(22-24).7.3 Lens SystemsInput lens systems are frequently em-ployed in CHA (and cylindrical sector) designs to vary thesurface analysis area (25) and to per
36、mit a convenient locationof the CHA so as to allow access of complementary surfacecharacterization techniques to the sample (26). The electro-static lens design often consists of a coaxial series of electrodesthat define the analysis area on the sample surface anddetermines the electron trajectories
37、 at the input to the analyzer.The lens system also determines the angular resolution andmodifies the transmission characteristics of the spectrometersystem (1). Reviews of electrostatic lens systems incorporatedin surface analysis instruments have been published (16-20,27). Lens systems have also be
38、en introduced at the exit ofanalyzers for photoelectron imaging (17, 28-30). Methods todetermine the specimen area examined are described in Prac-tice E1217.7.4 DetectorsDetection of the analyzed electrons is gen-erally accomplished through the use of an electron multiplier toproduce usable signals.
39、 Surface analysis instruments currentlyuse a variety of multipliers, but most are glass upon which aresistive coating is placed. The coating is formulated to providea substantial secondary electron yield upon primary electronimpact. The multiplier has a potential placed upon it so that thesecondary
40、electrons are accelerated to adjacent coated surfaces,thus providing the electron multiplying effect. Multipliers areavailable in various shapes for both analog and pulse countingamplification modes of operation (31). Single-channel electronmultipliers were common in early instruments, but multiple-
41、channel (“multichannel”) electron multipliers fabricated intothin plates are now available for use in detectors. See a generalreview of electron multipliers (32-35). The use of position-sensitive detectors, such as resistive anodes, as well as wedgeand strip anodes at the output of such electron mul
42、tipliers, hasafforded the ability to also record the spatial (angular) charac-teristics of the analyzed electrons and has thus permitted thedetermination of surface composition as a function of position(“chemical maps”) in XPS instruments (20, 33). A delay-linedetector has recently been developed fo
43、r XPS (34). Thedetection efficiency of single channel multipliers as a functionof incident energy, angle of incidence, as well as count ratehave been reported (35). In addition, the influence of thedetector electronics and counting systems have also beenexamined (36, 37).8. Keywords8.1 apertures; Au
44、ger electron spectroscopy; detectors; elec-tron spectrometers; electrostatic analyzers; lens systems; X-rayphotoelectron spectroscopyREFERENCES(1) Seah, M.P., and Smith, G.C., “Quantitative AES and XPS: Determi-nation of the Electron Spectrometer Transmission Function andDetector Sensitivity Energy
45、Dependencies for the Production of TrueElectron Emission Spectra in AES and XPS,” Surface and InterfaceAnalysis, Vol 15, 1990, pp. 751766.(2) Smith, G.C., and Seah, M.P., “Standard Reference Spectra for XPSand AES: Their Derivation, Validation and Use,” Surface and Inter-face Analysis, Vol 16, 1990,
46、 pp. 144148.(3) Seah, M.P., “XPS Reference Procedure for the Accurate IntensityCalibration of Electron SpectrometersResults of a BCR Intercom-parison Co-Sponsored by the VAMAS SCA TWA,” Surface andInterface Analysis, Vol 20, 1993, pp. 243266.(4) Seah, M.P.,“ A System for the Intensity Calibration of
47、 ElectronSpectrometers,” Journal of Electron Spectroscopy and RelatedPhenomenon, Vol 71, 1995, pp. 191204.(5) Seah, M. P., and Smith, G.C., “AES: Accurate Intensity Calibration ofElectron SpectrometersResults of a BCR Intercomparison Co-Sponsored by the VAMAS SCA TWA,” Surface and InterfaceAnalysis,
48、 Vol 17, 1991, pp. 855874.(6) Schweppe, J., Deslattes, R.D., Mooney, T., and Powell, C.J., “Accu-rate Measurement of Mg and Al K1,2X-Ray Energy Profiles,”Journal of Electron Spectroscopy and Related Phenomenon, Vol 67,1994, pp. 463478.(7) Seah, M.P., Gilmore, I.S., and Beamson, G., “XPS: Binding Ene
49、rgyCalibration of Electron Spectrometers: 5Re-evaluation of the Ref-erence Energies,” Surface Interface aNalysis, Vol 26, 1998, pp.642649.(8) Seah, M.P., and Gilmore, I.S., “AES: Energy Calibration of ElectronSpectrometers, III General Calibration Rules.” Journal of ELectronSpectroscopy and Related Phenomena, Vol 83, 1997, pp. 197208.(9) Seah, M.P., “AES: ebergy Calibration of Electron Spectrometers IV:Are-evaluation of the Reference ENergies,: Journal of ELectron Spec-trsocopy anf Related Phenomena, Vol 97, 1998, pp. 235241.(10) Seah
