ASTM E1016-07(2020)

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.
Designation: E1016 − 07 (Reapproved 2020)
Standard Guide for
Literature Describing Properties of Electrostatic Electron
Spectrometers
This standard is issued under the fixed designation E1016; 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 Spectrometers and Some X-Ray Photoelectron Spectrom-
eters
1.1 The purpose of this guide is to familiarize the analyst
E2108 Practice for Calibration of the Electron Binding-
with some of the relevant literature describing the physical
Energy Scale of an X-Ray Photoelectron Spectrometer
properties of modern electrostatic electron spectrometers.
2.2 ISO Standards:
1.2 Thisguideisintendedtoapplytoelectronspectrometers
ISO 18516 Surface Chemical Analysis—Auger Electron
generally used in Auger electron spectroscopy (AES) and
Spectroscopy and X-Ray Photoelectron Spectrsocopy—
X-ray photoelectron spectroscopy (XPS).
Determination of Lateral Resolution
1.3 The values stated in inch-pound units are to be regarded
ISO 21270 Surface Chemical Analysis—X-Ray Photoelec-
as standard. No other units of measurement are included in this tron and Auger Electron Spectrometers—Linearity of
standard.
Intensity Scale
ISO 24236 Surface Chemical Analysis—Auger Electron
1.4 This standard does not purport to address all of the
Spectroscopy—Repeatability and Constancy of Intensity
safety concerns, if any, associated with its use. It is the
Scale
responsibility of the user of this standard to establish appro-
ISO 24237 Surface Chemical Analysis—X-Ray Photoelec-
priate safety, health, and environmental practices and deter-
tron Spectroscopy—Repeatability and Constancy of In-
mine the applicability of regulatory limitations prior to use.
tensity Scale
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3. Terminology
ization established in the Decision on Principles for the
3.1 For definitions of terms used in this guide, refer to
Development of International Standards, Guides and Recom-
Terminology E673.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4. Summary of Guide
2. Referenced Documents
4.1 This guide serves as a resource for relevant literature
which describes the properties of electron spectrometers com-
2.1 ASTM Standards:
monly used in surface analysis.
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
2012)
5. Significance and Use
E902 Practice for Checking the Operating Characteristics of
X-Ray Photoelectron Spectrometers (Withdrawn 2011)
5.1 The analyst may use this document to obtain informa-
E1217 Practice for Determination of the Specimen Area tion on the properties of electron spectrometers and instrumen-
Contributing to the Detected Signal in Auger Electron
tal aspects associated with quantitative surface analysis.
6. General Description of Electron Spectrometers
This guide is under the jurisdiction of ASTM Committee E42 on Surface
6.1 An electron spectrometer is typically used to measure
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
the energy and angular distributions of electrons emitted from
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved Dec. 1, 2020. Published December 2020. Originally
a specimen, typically for energies in the range 0 to 2500 eV. In
ɛ1
approved in 1984. Last previous edition approved in 2012 as E1016 – 07 (2012) .
surface analysis applications, the analyzed electrons are pro-
DOI: 10.1520/E1016-07R20.
duced from the bombardment of a sample surface with
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’s Document Summary page on
the ASTM website. Available from International Organization for Standardization (ISO), ISO
The last approved version of this historical standard is referenced on Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
www.astm.org. Geneva, Switzerland, http://www.iso.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1016 − 07 (2020)
electrons, photons or ions. The entire spectrometer instrument 6.7 Specimen Area Contributing to the Detect Signal—See
may include one or more of the following: (1) apertures to Practice E1217 for methods to determine the specimen area
define the specimen area and emission solid angle for the contributing to the detected signal inAuger electron spectrom-
electrons accepted for analysis; (2) an electrostatic or magnetic eters and some X-Ray photoelectron spectrometers.
lens system, or both; (3) an electrostatic (dispersing) analyzer;
6.8 Calibration Protocol—Recommendations have been
and (4) a detector. Methods to check the operating character-
published describing spectrometer calibration requirements
istics of X-ray photoelectron spectrometers are reported in
and the frequency with which AES and XPS spectrometers
Practice E902.
should be calibrated (15).
6.2 Intensity Scale Calibration and Spectrometer Transmis-
sion Function—Quantitative analysis requires the determina-
7. Literature
tion of the ability of the spectrometer to transmit electrons, and
7.1 Electrostatic Analyzers—Spectrometers commonly used
the resultant detector signal, throughout the spectrometer
on modern AES and XPS spectrometer instruments generally
instrument. This can be described by an overall electron
employ electrostatic deflection analyzers.Auger electron spec-
energy-dependent transmission function Q(E) and is given by
trometersoftenusecylindricalmirroranalyzer(CMA)designs,
the product (1, 2), as follows:
although concentric hemispherical analyzers (CHA) (also
Q E 5 H E ·T E ·D E ·F E , (1)
~ ! ~ ! ~ ! ~ ! ~ !
known as spherical deflection (or sector) analyzers) are also
where:
used.The CHAdesign is the most common analyzer employed
on modern XPS instruments, although double-pass CMA
H(E) = the effect of mechanical imperfections (such as
designs were also employed on earlier XPS instruments.
aberrations, fringing fields, etc.),
T(E) = electron-optical transmission function, Retardingfieldanalyzers(RFA)havehistoricalinterestinearly
D(E) = detector efficiency, and AESwork,butarenowcommonlyusedonlowenergyelectron
F(E) = efficiency of the counting systems.
diffraction apparatus.
Knowledge of this transmission function permits the cali- 7.1.1 Electrostatic Deflection Analyzers—A review of the
brationofthespectraintensityaxis (3).Adetailedreviewofthe general properties of deflection analyzers may be found in
experimental determination of the transmission function for review articles (16, 17). More detailed reviews are also
XPS (4) and AES (5) measurements has been published.
available where, in addition to the CMA and CHA designs,
plane mirror, spherical mirror, cylindrical sector, and toroidal
6.3 Energy Scale Calibration—Calibration of the energy
deflection analyzers are treated (18-20).As the width of typical
scales of AES and XPS instruments is required for (1)
Auger spectral features are several electron volts, the use of a
meaningful comparison of building-energy or kinetic-energy
CMA design in conventional AES has sufficed for routine
measurements from two or more instruments; (2) valid identi-
analysis, particularly for small area analysis where a compro-
fication of chemical state from such comparisons; (3) effective
mise between signal-to-noise and energy resolution is impor-
use of databases containing reported energy values; and (4)as
tant. These are commonly used at a resolution defined by the
a component of a laboratory quality system. Suitable photon
full-width at half-maximum of the spectrometer energy
energyvaluesforAlandMganodeX-raysourcesoftenusedin
resolution, ∆E, divided by the electron energy, E, of 0.25 to
XPS measurements are available (6) and reference binding
0.6 %. The ability to incorporate an electron source concentric
energy values for copper (Cu), gold (Au), and silver (Ag) have
with the CMAaxis has been extensively exploited in scanning-
been published (7). Reference kinetic-energy values for Cu,
electron microscope instruments to give Auger data as a
aluminium (Al), and Au are also available (8, 9). Binding
function of beam position (that is, images). However, analysis
energy scale calibration procedures have been described in the
of the Auger spectra from some compounds and surface
literature for XPS (10, 11) and kinetic energy scale calibrations
morphologies may be enhanced by the use of a CHA design
for AES (8, 12-14) measurements. Practice E2108 describes a
which can provide better energy resolution (but a lower
procedure for calibrating the binding energy scale of XPS
transmission)andsuperiorangularresolution.TheCHAdesign
instruments using Cu, Ag, and Au specimens.
is most frequently employed on XPS instruments where
6.4 Linearity of Intensity Scale—See ISO 21270 for meth-
spectral features generally have narrow energy widths of 1 eV
ods to evaluate linearity of the intensity scale ofAES and XPS
or less and higher angular resolution is desired for the detected
spectrometers.
electrons than is possible with a CMA. The relationship
6.5 Repeatability and Constancy of Intensity Scale—See
between the pass energy of various spectrometer designs and
ISO 24236 and ISO 24237 for methods to evaluate the repeat-
the potential between their electrodes is described in detail
ability and constancy of intensity scales of AES and XPs
(16).
spectrometers, respectively.
7.1.2 Retarding Field Analyzers—The use of a retarding
6.6 Lateral Resolution—See ISO 18516 for methods to
field analyzer (RFA), consisting of concentric, spherical-sector
determine the lateral resolution of AES and XPS spectrom- grids, is currently used most commonly on electron diffraction
eters.
instruments where the angular distribution of the detected
electrons is examined. See also a brief review of RFA designs
(16)andasubstantialreportonresolutionandsensitivityissues
The boldface numbers in parentheses refer to the list of references at the end of
this guide. (21).
E1016 − 07 (2020)
7.2 Apertures—The effects of the spectrometer entrance and resistivecoatingisplaced.Thecoatingisformulatedtoprovide
exit slits and apertures, their associated fringing fields, as well a substantial secondary electron yield upon primary electron
as the effect of the divergence of the incident electron trajec- impact.The multiplier has a potential placed upon it so that the
tories on analyzer performance, particularly energy resolution, secondaryelectronsareacceleratedtoadjacentcoatedsurfaces,
havealsobeenreviewed (16-20).Adetailedexaminationofthe
thus providing the ele
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