1、Designation: E996 10Standard Practice forReporting Data in Auger Electron Spectroscopy and X-rayPhotoelectron Spectroscopy1This standard is issued under the fixed designation E996; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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 Auger and X-ray photoelectron spectra are obtainedusing a variety of excitation methods, analyzers, signal p
3、ro-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 The values stated in SI units are to be regarded asstan
4、dard. 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 appro-priate safety and health practices and determine the appl
5、ica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E673 Terminology Relating to Surface AnalysisE902 Practice for Checking the Operating Characteristics ofX-Ray Photoelectron SpectrometersE983 Guide for Minimizing Unwanted Electron Beam Ef-fects in Auger Ele
6、ctron SpectroscopyE995 Guide for Background Subtraction Techniques inAuger Electron Spectroscopy and X-ray PhotoelectronSpectroscopyE1078 Guide for Specimen Preparation and Mounting inSurface AnalysisE1127 Guide for Depth Profiling in Auger Electron Spec-troscopy3. Terminology3.1 DefinitionsFor defi
7、nitions of terms used in this guide,refer to Terminology E673.4. Summary of Practice4.1 Report all experimental conditions 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 exper
8、imental conditions under which spectraare taken in the “Experiment” section of all reports andpublications.5.2 Identify 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
9、 the figure caption.6. Information To Be Reported6.1 Equipment Used:6.1.1 If a commercial electron spectroscopy system 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 generati
10、ng theexperimental data, such as a sputter ion source.6.1.2 If a spectrometer system has been assembled fromseveral 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 softw
11、are packages used to acquire or process thedata.6.2 Specimen Analyzed:6.2.1 Describe the specimen as completely as possible, 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 positionin
12、g thespecimen for analysis, for example, mounted on a carousel, ormounted between strips of a particular metal. If the specimenis heated, cooled or treated in the spectrometer system,describe the method used (for example, heated by electron1This practice is under the jurisdiction of ASTM Committee E
13、42 on SurfaceAnalysis and is the direct responsibility of Subcommittee E42.03 on Auger ElectronSpectroscopy and X-Ray Photoelectron Spectroscopy.Current edition approved Nov. 1, 2010. Published December 2010. Originallyapproved in 1984. Last previous edition approved in 2004 as E996 04. DOI:10.1520/
14、E0996-10.2For 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.1Copyright ASTM International, 100 Barr Harbor Drive
15、, PO Box C700, West Conshohocken, PA 19428-2959, United States.bombardment on the back of the specimen, or resistivelyheated). See Guide E1078 for more detail.6.2.3 State the operating pressure of the vacuum systemduring data acquisition and the position of the vacuum gagerelative to the specimen be
16、ing analyzed. State if the system wasbackfilled with a sputter gas. Indicate the presence of activegases if they are appropriate to 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 Analys
17、is:6.3.1 Excitation SourceFor electron beam excitation, statethe beam energy, beam size, incident current, whether the beamis stationary or scanned (if scanned, state the area), and angleof incidence. State the method used to determine the electronbeam diameter. (See Note 1.) For radiation-sensitive
18、 speci-mens, give the pre-analysis and analysis beam exposure times.See Guide E983 to minimize unwanted electron beam effects.For X-ray excitation, specify the anode material, characteristicradiation energy, beam size at the specimen, whether the beamis stationary or scanned (if scanned, state the a
19、rea), sourcestrength, electron emission current, acceleration voltage, win-dow material, and whether the source X-ray was monochro-matic.NOTE 1The common method of measuring incident electron beamcurrent by applying a low (approximately + 100 volt) specimen bias doesnot account for emission of backs
20、cattered 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 necessary to correct for the charging of the specimenunder irradiation. When energies of lines from s
21、uch 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 current density should also be given.6.3.3 AnalyzerState the type of analyzer (and lens) usedfor elec
22、tron collection (cylindrical mirror (single or double-pass), hemispherical, spherical, and the like). State the spec-trometers energy resolution, retardation ratio, pass energy (ifpertinent), emission angle, source-to-analyzer angle, accep-tance angle width, and specimen acceptance area. Describehow
23、 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 should be stated. If electron beam modula-tion is used, the electron beam chopping frequency and dutycycle
24、 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,recorder, or digitizing system.6.3.6 Scan RateIf an analog scan is used, give the sweeprate in eV/s (electro
25、nvolt/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. It isrecommended that the procedure described in Practice E902 beused to ensure that the spectromete
26、r is operating in a repro-ducible manner.6.3.8 Detector DescriptionDescribe the detector used. Ifan electron multiplier is used and the front is biased, state thebias voltage. Indicate whether the output of the analyzer ismeasured directly, or by a voltage isolation method, by pulsecounting, or by v
27、oltage-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,state the number of scans.6.3.10 SputteringIf ion sputtering was used for cleaningor sputter depth pr
28、ofiling, 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 used, state the area and rate.State the total pressure in the vicinity of the specimen (ifknown) and
29、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 relative sputter rates be determined usinga known thickness of tantalum pentoxide or silicon dioxide.
30、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 E995), deconvolu-tions, curve resolution, intensity scale correction, satellitesubtraction, or other processing of
31、 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 eachmethod should be explained.6.4.2 QuantificationIf the elemental concentrations orsurface coverages ar
32、e calculated from the data, indicate themethod, type of software, and version, along with the valuesand source of any parameters, for example, relative sensitivityfactors, elemental region end points used for peak area, orintensity determination, and instrument transmission functioncorrection coeffi
33、cients. State the signal-to-noise ratio, preci-sion, and minimum detection limits 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 excur
34、sion in the dN/dE-typespectrum is reported. When peak 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
35、, give an estimate of theprecision of the measurement.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/dEE996 102if the first derivative is measured. With cer
36、tain types ofanalyzers, other electron energy distributions are 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 th
37、e units as “counts” or(preferred) “counts per second.”6.5.2 Sputter 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 “peakheight” or “peak area” as applicable, or in the case ofderi
38、vative spectra “peak-to-peak height.” Label the horizontalaxis “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 E1127.6.5.3 Line ScansThe vertical axis of the data should belabeled similarly to that
39、for sputter depth profiles, in 6.5.2.Note the kinetic 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
40、 and specimen topography have beenminimized by plotting 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, millime
41、tres, etc.6.5.4 MapsDescribe the Auger or XPS signal used 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,descr
42、ibe and display the intensity scale (dot intensity, graylevels, 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(pix
43、els) being used in the horizontal and vertical direction.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
44、the full reporting of all information necessary to describethe 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
45、, energy, strength, and angle ofincidence,7.1.3 Analyzer 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 a
46、cquisition time, and modula-tion amplitude (for phase-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 t
47、his standard. Users of this standard are expressly advised 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
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49、sponsible technical committee, which you may attend. If 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. Individual 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 A
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