1、Designation: E 996 04Standard Practice forReporting Data in Auger Electron Spectroscopy and X-rayPhotoelectron Spectroscopy1This standard is issued under the fixed designation E 996; 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 Auger and x-ray photoelectron spectra are obtainedusing a variety of excitation methods, analyzers, signa
3、l pro-cessing, and digitizing techniques.1.2 This practice lists the desirable information that shall bereported to fully describe the experimental conditions, speci-men conditions, data recording procedures, and data transfor-mation processes.1.3 This standard does not purport to address all of the
4、safety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 673 Terminology Relating t
5、o Surface AnalysisE 902 Practice for Checking the Operating Characteristicsof X-Ray Photoelectron SpectrometersE 983 Guide for Minimizing Unwanted Electron BeamEffects in Auger Electron SpectroscopyE 995 Guide for Background Subtraction Techniques inAuger Electron Spectroscopy and X-Ray Photoelectro
6、nSpectroscopyE 1078 Guide for Specimen Preparation and Mounting inSurface AnalysisE 1127 Guide for Depth Profiling in Auger Electron Spec-troscopy3. Terminology3.1 DefinitionsFor definitions of terms used in this guide,refer to Terminology E 673.4. Summary of Practice4.1 Report all experimental cond
7、itions that affect Auger andx-ray photoelectron spectra so spectra can be reproduced inother laboratories or be compared with other spectra.5. Significance and Use5.1 Include the experimental conditions under which spectraare taken in the “Experiment” section of all reports andpublications.5.2 Ident
8、ify any parameters that are changed between dif-ferent spectra in the “Experiment” section of publications andreports, and include the specific parameters applicable to eachspectrum in the figure caption.6. Information To Be Reported6.1 Equipment Used:6.1.1 If a commercial electron spectroscopy syst
9、em is used,specify the manufacturer and model. Indicate the type ofelectron excitation source and electron analyzer as well as themodel designation of other equipment used for generating theexperimental data, such as a sputter ion source.6.1.2 If a spectrometer system has been assembled fromseveral
10、components specify the manufacturers and modelnumbers of excitation source, analyzer, and auxiliary equip-ment.6.1.3 Identify the model name, version number, and manu-facturer of software packages used to acquire or process thedata.6.2 Specimen Analyzed:6.2.1 Describe the specimen as completely as p
11、ossible, forexample, its bulk composition, history, any methods of clean-ing or sectioning pre-analysis treatments, and dimensions.6.2.2 Describe the method of mounting and positioning thespecimen for analysis, for example, mounted on a carousel, ormounted between strips of a particular metal. If th
12、e specimenis heated, cooled or treated in the spectrometer system,describe the method used (for example, heated by electronbombardment on the back of the specimen, or resistivelyheated). See Guide E 1078 for more detail.1This practice is under the jurisdiction of ASTM Committee E42 on SurfaceAnalysi
13、s and is the direct responsibility of Subcommittee E42.03 on Auger ElectronSpectroscopy and X-Ray Photoelectron Spectroscopy.Current edition approved Nov. 1, 2004. Published December 2004. Originallyapproved in 1984. Last previous edition approved in 1999 as E 996 94 (1999).2For referenced ASTM stan
14、dards, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,
15、PA 19428-2959, United States.6.2.3 State the operating pressure of the vacuum systemduring data acquisition and the position of the vacuum gagerelative to the specimen being analyzed. State if the system wasbackfilled with a sputter gas. Indicate the presence of activegases if they are appropriate t
16、o the measurement. If the system(and specimen) was baked-out before analysis, the time,temperature and final pressure should also be stated.6.3 Parameters Used for Analysis:6.3.1 Excitation SourceFor electron beam excitation, statethe beam energy, beam size, incident current, whether the beamis stat
17、ionary or scanning (if scanning, state the area), and angleof incidence. State the method used to determine the electronbeam diameter. (See Note 1.) For radiation-sensitive speci-mens, give the pre-analysis and analysis beam exposure times.See Guide E 983 to minimize unwanted electron beam effects.F
18、or x-ray excitation, specify the anode material, characteristicradiation energy, beam size at the specimen, source strength,electron emission current, acceleration voltage, window mate-rial, and whether the source x-ray was monochromatic.NOTE 1The common method of measuring incident electron beamcur
19、rent by applying a low (approximately + 100 volt) specimen bias doesnot account for emission of backscattered electrons. The preferred methodis to use a Faraday cup bearing a small entrance aperture to limit thenumber of electrons escaping.6.3.2 Charge CorrectionFor insulating specimens, it isoften
20、necessary to correct for the charging of the specimenunder irradiation. When energies of lines from such specimensare quoted, the method of charge correction must also bedescribed as well as the standard value assumed. If an electronbeam or ion beam is used, its beam current, energy, anddiameter or
21、current density should also be given.6.3.3 AnalyzerState the type of analyzer (and lens) usedfor electron collection (cylindrical mirror (single or double-pass), hemispherical, spherical, and the like). State the spec-trometers energy resolution, retardation ratio, pass energy (ifpertinent), emissio
22、n angle, source-to-analyzer angle, accep-tance angle width, and specimen acceptance area. Describehow any of these analyzer properties vary with electron energy.6.3.4 ModulationIf phase-sensitive detection is used toobtain the Auger spectrum in derivative form the peak-to-peakenergy modulation shoul
23、d be stated. If electron beam modula-tion is used, the electron beam chopping frequency and dutycycle should be stated.6.3.5 Time ConstantGive the system time constant ifanalog detection is used. The limiting time constant could bedetermined by that of the phase-sensitive detector, ratemeter,recorde
24、r, or digitizing system.6.3.6 Scan RateIf an analog scan is used, give the sweeprate in eV/s (electronvolt/second). If a stepped scan is used,give the step size in eV and the dwell time per step.6.3.7 Energy Scale CalibrationThe method for calibra-tion of the binding energy scale shall be specified.
25、 It isrecommended that the procedure described in Practice E 902be used to ensure that the spectrometer is operating in areproducible manner.6.3.8 Detector DescriptionDescribe the detector used. Ifan electron multiplier is used and the front is bias, state the biasvoltage. Indicate whether the outpu
26、t of the analyzer is mea-sured directly, or by a voltage isolation method, by pulsecounting, or by voltage-to-frequency conversion. For a multi-channel detector, give the number of channels in the spectrumcovered by the width of the detector.6.3.9 Signal AveragingIf the spectrum is signal averaged,s
27、tate the number of scans.6.3.10 SputteringIf ion sputtering was used for cleaningor sputter depth profiling, describe the ion species, ion energy,energy filtering, neutral rejection (if employed), the beamcurrent, diameter, or maximum current density, and angle ofincidence. If ion beam scanning is u
28、sed, state the area and rate.State the total pressure in the vicinity of the specimen (ifknown) and if the sputtering source was differentially pumped.If a depth scale is given on a sputter depth profile, state themethod of depth calibration. If the sputter rate is not known, itis recommended that r
29、elative sputter rates be determined usinga known thickness of tantalum pentoxide or silicon dioxide.State the specimen rotation rate if rotational depth profilingwas used.6.4 Data Handling:6.4.1 Data ProcessingDescribe any smoothing, differen-tiation, background subtraction (see Guide E 995), deconv
30、olu-tions, curve resolution, intensity scale correction, satellitesubtraction, or other processing of the data. Specify anyassumptions and approximations required for the processing,together with the data reduction algorithm. In the case ofmultiple processing methods, the step-by-step effect of each
31、method should be explained.6.4.2 QuantificationIf the elemental concentrations orsurface coverages are calculated from the data, indicate themethod and model used, along with the values and source ofany parameters, for example relative sensitivity factors. Statethe signal-to-noise ratio, precision,
32、and minimum detectionlimits of the data.6.4.3 Peak EnergiesAuger electron and photoelectronpeak positions are normally reported as the energy of maxi-mum intensity in the N(E)-type spectrum. For derivative Augerspectra, the maximum negative excursion in the dN/dE-typespectrum is reported. When peak
33、energies are reported, alsoreport the peak energies of any calibration materials used tocheck the spectrometer performance. When line energies arecited more precisely than 0.1 eV, describe the method used todetermine the peak energy. For all data, give an estimate of theprecision of the measurement.
34、6.5 Display of Data:6.5.1 Auger and XPS SpectraThe horizontal electronenergy scale shall be marked in eV. Mark the vertical axis asN(E) if the electron energy distribution is measured, or dN/dEif the first derivative is measured. With certain types ofanalyzers, other electron energy distributions ar
35、e measured andthese should be given, for example, with a single-pass cylin-drical mirror analyzer EN(E), or dEN(E)/dE, are usuallymeasured. The units used for the vertical axis can be “arbitraryunits.” If pulse counting is used, report the units as “counts” or(preferred) “counts per second.”6.5.2 Sp
36、utter Depth ProfilesThe signal intensity (in arbi-trary units) or the atomic percent concentration are given on thevertical axis. If signal intensity is used, label the axis “peakE996042height” or “peak area” as applicable, or in the case ofderivative spectra “peak-to-peak height.” Label the horizon
37、talaxis “depth,” if this is known, otherwise use “sputter time.”Report sputtering conditions as in 6.3.10. More detail on depthprofiling is provided in Guide E 1127.6.5.3 Line ScansThe vertical axis of the data should belabeled similarly to that for sputter depth profiles, in 6.5.2.Note the kinetic
38、energy used for making the measurement.State if one energy is used, or if intensity is calculated as PB(or a linear background intensity interpolated between twobackground values, or some other means). Note if the effects ofelectron current drift and specimen topography have beenminimized by plottin
39、g such functions as:P 2 B!/B or P 2 B!/P 1 B! (1)where:P = a measure of the signal intensity, andB = the background intensity at an energy offset from thepeak.3Label the horizontal axis “position” with the appropriateunits in micrometres, millimetres, etc.6.5.4 MapsDescribe the Auger or XPS signal u
40、sed forobtaining a map of an element or chemical state (see 6.5.3).Mark the magnification scale on the map by including adimension marker (m or nm). Indicate the type of signal (see6.5.1) used for determining the brightness of the map. Also,describe and display the intensity scale (dot intensity, gr
41、aylevels, or false colors) used to produce the map. Indicate iftopography correction was used (6.5.3) or other mathematicalprocessing techniques, such as smoothing. If digital images arebeing presented, indicate the number of picture elements(pixels) being used in the horizontal and vertical directi
42、on.Also indicate the mapping time, beam current, and number ofintensity levels. Also indicate if thresholding or non-linearprocessing has been applied.7. Abbreviated Reporting of Data7.1 For some publications and reports, space does not allowfor the full reporting of all information necessary to des
43、cribethe measurement and data. While the analyst needs to have thefull measurement description available, reporting the followingminimum parameters may satisfy many requirements:7.1.1 Instrument manufacturer and model:7.1.2 Excitation source type, energy, strength, and angle ofincidence,7.1.3 Analyz
44、er and lens type, nominal energy resolution (aspercent for fixed retardation ratio or as eV for fixed analyzertransmission), angle of emission, calibration energies (if any);7.1.4 Sampling area on the specimen, and7.1.5 Step scan interval, data acquisition time, and modula-tion amplitude (for phase-
45、sensitive detection).8. Keywords8.1 Auger electron spectroscopy; surface analysis; X-rayphotoelectron spectroscopyASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly adv
46、ised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either
47、 reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. I
48、f you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Indivi
49、dual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).3Prutton, M., Larson, L. A., and Poppa, H., Journal of Applied Physics, Vol 54,1983, p. 374.E996043
