ASTM E996-10(2018)
(Practice)Standard Practice for Reporting Data in Auger Electron Spectroscopy and X-ray Photoelectron Spectroscopy
Standard Practice for Reporting Data in Auger Electron Spectroscopy and X-ray Photoelectron Spectroscopy
SIGNIFICANCE AND USE
5.1 Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.
5.2 Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: E996 − 10 (Reapproved 2018)
Standard Practice for
Reporting Data in Auger Electron Spectroscopy and X-ray
Photoelectron Spectroscopy
This standard is issued under the fixed designation E996; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope E983 Guide for Minimizing Unwanted Electron Beam Ef-
fects in Auger Electron Spectroscopy
1.1 Auger and X-ray photoelectron spectra are obtained
E995 Guide for Background Subtraction Techniques in Au-
using a variety of excitation methods, analyzers, signal
ger Electron Spectroscopy and X-Ray Photoelectron
processing, and digitizing techniques.
Spectroscopy
1.2 This practice lists the desirable information that shall be
E1078 Guide for Specimen Preparation and Mounting in
reported to fully describe the experimental conditions, speci-
Surface Analysis
men conditions, data recording procedures, and data transfor-
E1127 Guide for Depth Profiling in Auger Electron Spec-
mation processes.
troscopy
1.3 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions—For definitions of terms used in this
standard.
practice, refer to Terminology E673.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Practice
responsibility of the user of this standard to establish appro-
4.1 Report all experimental conditions that affectAuger and
priate safety, health, and environmental practices and deter-
X-ray photoelectron spectra so spectra can be reproduced in
mine the applicability of regulatory limitations prior to use.
other laboratories or be compared with other spectra.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard- 5. Significance and Use
ization established in the Decision on Principles for the
5.1 Includetheexperimentalconditionsunderwhichspectra
Development of International Standards, Guides and Recom-
are taken in the “Experiment” section of all reports and
mendations issued by the World Trade Organization Technical
publications.
Barriers to Trade (TBT) Committee.
5.2 Identify any parameters that are changed between dif-
ferent spectra in the “Experiment” section of publications and
2. Referenced Documents
reports, and include the specific parameters applicable to each
2.1 ASTM Standards:
spectrum in the figure caption.
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
2012)
6. Information To Be Reported
E902 Practice for Checking the Operating Characteristics of
6.1 Equipment Used:
X-Ray Photoelectron Spectrometers (Withdrawn 2011)
6.1.1 If a commercial electron spectroscopy system is used,
specify the manufacturer and model. Indicate the type of
electron excitation source and electron analyzer as well as the
This practice is under the jurisdiction of ASTM Committee E42 on Surface
model designation of other equipment used for generating the
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
Spectroscopy and X-Ray Photoelectron Spectroscopy. experimental data, such as a sputter ion source.
Current edition approved Nov. 1, 2018. Published November 2018. Originally
6.1.2 If a spectrometer system has been assembled from
approved in 1984. Last previous edition approved in 2010 as E996–10. DOI:
several components specify the manufacturers and model
10.1520/E0996–10R18.
numbers of excitation source, analyzer, and auxiliary equip-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ment.
Standards volume information, refer to the standard’s Document Summary page on
6.1.3 Identify the model name, version number, and manu-
the ASTM website.
3 facturer of software packages used to acquire or process the
The last approved version of this historical standard is referenced on
www.astm.org. data.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E996 − 10 (2018)
6.2 Specimen Analyzed: determined by that of the phase-sensitive detector, ratemeter,
6.2.1 Describe the specimen as completely as possible, for recorder, or digitizing system.
example, its bulk composition, history, any methods of clean-
6.3.6 Scan Rate—If an analog scan is used, give the sweep
ing or sectioning, pre-analysis treatments, and dimensions.
rate in eV/s (electronvolt/second). If a stepped scan is used,
6.2.2 Describe the method of mounting and positioning the
give the step size in eV and the dwell time per step.
specimen for analysis, for example, mounted on a carousel, or
6.3.7 EnergyScaleCalibration—Themethodforcalibration
mounted between strips of a particular metal. If the specimen
of the binding energy scale shall be specified. It is recom-
is heated, cooled or treated in the spectrometer system,
mended that the procedure described in Practice E902 be used
describe the method used (for example, heated by electron
to ensure that the spectrometer is operating in a reproducible
bombardment on the back of the specimen, or resistively
manner.
heated). See Guide E1078 for more detail.
6.3.8 Detector Description—Describe the detector used. If
6.2.3 State the operating pressure of the vacuum system
an electron multiplier is used and the front is biased, state the
during data acquisition and the position of the vacuum gage
bias voltage. Indicate whether the output of the analyzer is
relativetothespecimenbeinganalyzed.Stateifthesystemwas
measured directly, or by a voltage isolation method, by pulse
backfilled with a sputter gas. Indicate the presence of active
counting, or by voltage-to-frequency conversion. For a multi-
gases if they are appropriate to the measurement. If the system
channel detector, give the number of channels in the spectrum
(and specimen) was baked-out before analysis, the time,
covered by the width of the detector.
temperature and final pressure should also be stated.
6.3.9 Signal Averaging—If the spectrum is signal averaged,
6.3 Parameters Used for Analysis:
state the number of scans.
6.3.1 ExcitationSource—For electron beam excitation, state
6.3.10 Sputtering—If ion sputtering was used for cleaning
thebeamenergy,beamsize,incidentcurrent,whetherthebeam
or sputter depth profiling, describe the ion species, ion energy,
is stationary or scanned (if scanned, state the area), and angle
energy filtering, neutral rejection (if employed), the beam
of incidence. State the method used to determine the electron
current, diameter, or maximum current density, and angle of
beam diameter. (See Note 1.) For radiation-sensitive
incidence. If ion beam scanning is used, state the area and rate.
specimens, give the pre-analysis and analysis beam exposure
State the total pressure in the vicinity of the specimen (if
times. See Guide E983 to minimize unwanted electron beam
known) and if the sputtering source was differentially pumped.
effects. For X-ray excitation, specify the anode material,
If a depth scale is given on a sputter depth profile, state the
characteristic radiation energy, beam size at the specimen,
method of depth calibration. If the sputter rate is not known, it
whether the beam is stationary or scanned (if scanned, state the
is recommended that relative sputter rates be determined using
area), source strength, electron emission current, acceleration
a known thickness of tantalum pentoxide or silicon dioxide.
voltage, window material, and whether the source X-ray was
State the specimen rotation rate if rotational depth profiling
monochromatic.
was used.
NOTE 1—The common method of measuring i
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E996 − 10 E996 − 10 (Reapproved 2018)
Standard Practice for
Reporting Data in Auger Electron Spectroscopy and X-ray
Photoelectron Spectroscopy
This standard is issued under the fixed designation E996; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and
digitizing techniques.
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen
conditions, data recording procedures, and data transformation processes.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
E673 Terminology Relating to Surface Analysis (Withdrawn 2012)
E902 Practice for Checking the Operating Characteristics of X-Ray Photoelectron Spectrometers (Withdrawn 2011)
E983 Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy
E995 Guide for Background Subtraction Techniques in Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy
E1078 Guide for Specimen Preparation and Mounting in Surface Analysis
E1127 Guide for Depth Profiling in Auger Electron Spectroscopy
3. Terminology
3.1 Definitions—For definitions of terms used in this guide,practice, refer to Terminology E673.
4. Summary of Practice
4.1 Report all experimental conditions that affect Auger and X-ray photoelectron spectra so spectra can be reproduced in other
laboratories or be compared with other spectra.
5. Significance and Use
5.1 Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and
publications.
5.2 Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports,
and include the specific parameters applicable to each spectrum in the figure caption.
This practice is under the jurisdiction of ASTM Committee E42 on Surface Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved Nov. 1, 2010Nov. 1, 2018. Published December 2010November 2018. Originally approved in 1984. Last previous edition approved in 20042010
as E996 – 04.E996–10. DOI: 10.1520/E0996-10.10.1520/E0996–10R18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E996 − 10 (2018)
6. Information To Be Reported
6.1 Equipment Used:
6.1.1 If a commercial electron spectroscopy system is used, specify the manufacturer and model. Indicate the type of electron
excitation source and electron analyzer as well as the model designation of other equipment used for generating the experimental
data, such as a sputter ion source.
6.1.2 If a spectrometer system has been assembled from several components specify the manufacturers and model numbers of
excitation source, analyzer, and auxiliary equipment.
6.1.3 Identify the model name, version number, and manufacturer of software packages used to acquire or process the data.
E996 − 10 (2018)
6.2 Specimen Analyzed:
6.2.1 Describe the specimen as completely as possible, for example, its bulk composition, history, any methods of cleaning or
sectioning, pre-analysis treatments, and dimensions.
6.2.2 Describe the method of mounting and positioning the specimen for analysis, for example, mounted on a carousel, or
mounted between strips of a particular metal. If the specimen is heated, cooled or treated in the spectrometer system, describe the
method used (for example, heated by electron bombardment on the back of the specimen, or resistively heated). See Guide E1078
for more detail.
6.2.3 State the operating pressure of the vacuum system during data acquisition and the position of the vacuum gage relative
to the specimen being analyzed. State if the system was backfilled with a sputter gas. Indicate the presence of active gases 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 Analysis:
6.3.1 Excitation Source—For electron beam excitation, state the beam energy, beam size, incident current, whether the beam is
stationary or scanned (if scanned, state the area), and angle of incidence. State the method used to determine the electron beam
diameter. (See Note 1.) For radiation-sensitive specimens, 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, characteristic radiation energy, beam
size at the specimen, whether the beam is stationary or scanned (if scanned, state the area), source strength, electron emission
current, acceleration voltage, window material, and whether the source X-ray was monochromatic.
NOTE 1—The common method of measuring incident electron beam current by applying a low (approximately + 100 volt) specimen bias does not
account for emission of backscattered electrons. The preferred method is to use a Faraday cup bearing a small entrance aperture to limit the number of
electrons escaping.
6.3.2 Charge Correction—For insulating specimens, it is often necessary to correct for the charging of the specimen under
irradiation. When energies of lines from such specimens are quoted, the method of charge correction must also be described as well
as the standard value assumed. If an electron beam or ion beam is used, its beam current, energy, and diameter or current density
should also be given.
6.3.3 Analyzer—State the type of analyzer (and lens) used for electron collection (cylindrical mirror (single or double-pass),
hemispherical, spherical, and the like). State the spectrometer’s energy resolution, retardation ratio, pass energy (if pertinent),
emission angle, source-to-analyzer angle, acceptance angle width, and specimen acceptance area. Describe how any of these
analyzer properties vary with electron energy.
6.3.4 Modulation—If phase-sensitive detection is used to obtain the Auger spectrum in derivative form the peak-to-peak energy
modulation should be stated. If electron beam modulation is used, the electron beam chopping frequency and duty cycle should
be stated.
6.3.5 Time Constant—Give the system time constant if analog detection is used. The limiting time constant could be determined
by that of the phase-sensitive detector, ratemeter, recorder, or digitizing system.
6.3.6 Scan Rate—If an analog scan is use
...
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