ASTM E1016-07(2012)e1
(Guide)Standard Guide for Literature Describing Properties of Electrostatic Electron Spectrometers
Standard Guide for Literature Describing Properties of Electrostatic Electron Spectrometers
SIGNIFICANCE AND USE
The analyst may use this document to obtain information on the properties of electron spectrometers and instrumental aspects associated with quantitative surface analysis.
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with some of the relevant literature describing the physical properties of modern electrostatic electron spectrometers.
1.2 This guide is intended to apply to electron spectrometers generally used in Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).
1.3 The values stated in inch-pound 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 and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: E1016 − 07 (Reapproved 2012)
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.
ε NOTE—Editorial corrections were made throughout in November 2012.
1. Scope 2.2 ISO Standards:
ISO 18516 Surface Chemical Analysis—Auger Electron
1.1 The purpose of this guide is to familiarize the analyst
Spectroscopy and X-Ray Photoelectron Spectrsocopy—
with some of the relevant literature describing the physical
Determination of Lateral Resolution
properties of modern electrostatic electron spectrometers.
ISO 21270 Surface Chemical Analysis—X-Ray Photoelec-
1.2 Thisguideisintendedtoapplytoelectronspectrometers
tron and Auger Electron Spectrometers—Linearity of
generally used in Auger electron spectroscopy (AES) and
Intensity Scale
X-ray photoelectron spectroscopy (XPS).
ISO 24236 Surface Chemical Analysis—Auger Electron
1.3 The values stated in inch-pound units are to be regarded Spectroscopy—Repeatability and Constancy of Intensity
Scale
as standard. No other units of measurement are included in this
standard. ISO 24237 Surface Chemical Analysis—X-Ray Photoelec-
tron Spectroscopy—Repeatability and Constancy of In-
1.4 This standard does not purport to address all of the
tensity Scale
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 For definitions of terms used in this guide, refer to
bility of regulatory limitations prior to use.
Terminology E673.
2. Referenced Documents
4. Summary of Guide
2.1 ASTM Standards:
4.1 This guide serves as a resource for relevant literature
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
which describes the properties of electron spectrometers com-
2012)
monly used in surface analysis.
E902 Practice for Checking the Operating Characteristics of
X-Ray Photoelectron Spectrometers (Withdrawn 2011)
5. Significance and Use
E1217 Practice for Determination of the Specimen Area
5.1 The analyst may use this document to obtain informa-
Contributing to the Detected Signal in Auger Electron
Spectrometers and Some X-Ray Photoelectron Spectrom- tion on the properties of electron spectrometers and instrumen-
tal aspects associated with quantitative surface analysis.
eters
E2108 Practice for Calibration of the Electron Binding-
6. General Description of Electron Spectrometers
Energy Scale of an X-Ray Photoelectron Spectrometer
6.1 An electron spectrometer is typically used to measure
the energy and angular distributions of electrons emitted from
This guide is under the jurisdiction of ASTM Committee E42 on Surface
a specimen, typically for energies in the range 0 to 2500 eV. In
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
surface analysis applications, the analyzed electrons are pro-
Spectroscopy and X-Ray Photoelectron Spectroscopy.
duced from the bombardment of a sample surface with
Current edition approved Nov. 1, 2012. Published December 2012. Originally
approved in 1984. Last previous edition approved in 2007 as E1016 – 07. DOI: electrons, photons or ions. The entire spectrometer instrument
10.1520/E1016-07R12E01.
may include one or more of the following: (1) apertures to
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
define the specimen area and emission solid angle for the
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.
3 4
The last approved version of this historical standard is referenced on Available from International Organization for Standardization (ISO), 1 rue de
www.astm.org. Varembé, 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 19428-2959. United States
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E1016 − 07 (2012)
electrons accepted for analysis; (2) an electrostatic or magnetic contributing to the detected signal inAuger electron spectrom-
lens system, or both; (3) an electrostatic (dispersing) analyzer; eters and some X-Ray photoelectron spectrometers.
and (4) a detector. Methods to check the operating character-
6.8 Calibration Protocol—Recommendations have been
istics of X-ray photoelectron spectrometers are reported in
published describing spectrometer calibration requirements
Practice E902.
and the frequency with which AES and XPS spectrometers
6.2 Intensity Scale Calibration and Spectrometer Transmis-
should be calibrated (15).
sion Function—Quantitative analysis requires the determina-
tion of the ability of the spectrometer to transmit electrons, and
7. Literature
the resultant detector signal, throughout the spectrometer
7.1 Electrostatic Analyzers—Spectrometers commonly used
instrument. This can be described by an overall electron
on modern AES and XPS spectrometer instruments generally
energy-dependent transmission function Q(E) and is given by
employ electrostatic deflection analyzers.Auger electron spec-
the product (1, 2), as follows:
trometersoftenusecylindricalmirroranalyzer(CMA)designs,
Q~E! 5 H~E!·T~E!·D~E!·F~E!, (1)
although concentric hemispherical analyzers (CHA) (also
known as spherical deflection (or sector) analyzers) are also
where:
used.The CHAdesign is the most common analyzer employed
H(E) = the effect of mechanical imperfections (such as
on modern XPS instruments, although double-pass CMA
aberrations, fringing fields, etc.),
designs were also employed on earlier XPS instruments.
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,
6.3 Energy Scale Calibration—Calibration of the energy
plane mirror, spherical mirror, cylindrical sector, and toroidal
scales of AES and XPS instruments is required for (1)
deflection analyzers are treated (18-20).As the width of typical
meaningful comparison of building-energy or kinetic-energy
Auger spectral features are several electron volts, the use of a
measurements from two or more instruments; (2) valid identi-
CMA design in conventional AES has sufficed for routine
fication of chemical state from such comparisons; (3) effective
analysis, particularly for small area analysis where a compro-
use of databases containing reported energy values; and (4)as
mise between signal-to-noise and energy resolution is impor-
a component of a laboratory quality system. Suitable photon
tant. These are commonly used at a resolution defined by the
energyvaluesforAlandMganodeX-raysourcesoftenusedin
full-width at half-maximum of the spectrometer energy
XPS measurements are available (6) and reference binding
resolution, ∆E, divided by the electron energy, E, of 0.25 to
energy values for copper (Cu), gold (Au), and silver (Ag) have
0.6 %. The ability to incorporate an electron source concentric
been published (7). Reference kinetic-energy values for Cu,
with the CMAaxis has been extensively exploited in scanning-
aluminium (Al), and Au are also available (8, 9). Binding
electron microscope instruments to give Auger data as a
energy scale calibration procedures have been described in the
function of beam position (that is, images). However, analysis
literature for XPS (10, 11) and kinetic energy scale calibrations
of the Auger spectra from some compounds and surface
for AES (8, 12-14) measurements. Practice E2108 describes a
morphologies may be enhanced by the use of a CHA design
procedure for calibrating the binding energy scale of XPS
which can provide better energy resolution (but a lower
instruments using Cu, Ag, and Au specimens.
transmission)andsuperiorangularresolution.TheCHAdesign
6.4 Linearity of Intensity Scale—See ISO 21270 for meth- is most frequently employed on XPS instruments where
ods to evaluate linearity of the intensity scale ofAES and XPS
spectral features generally have narrow energy widths of 1 eV
spectrometers. or less and higher angular resolution is desired for the detected
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
6.7 Specimen Area Contributing to the Detect Signal—See
electrons is examined. See also a brief review of RFA designs
Practice E1217 for methods to determine the specimen area
(16)andasubstantialreportonresolutionandsensitivityissues
(21).
7.2 Apertures—The effects of the spectrometer entrance and
The boldface numbers in parentheses refer to the list of references at the end of
this guide. exit slits and apertures, their associated fringing fields, as well
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E1016 − 07 (2012)
as the effect of the divergence of the incident electron trajec- a substantial secondary electron yield upon primary electron
tories on analyzer performance, particularly energy resolution, impact.The multiplier has a potential placed upon it so that the
havealsobeenreviewed (16-20).Adetailedexaminationofthe secondaryelectronsareacceleratedtoadjacentcoatedsurfaces,
effects of unwanted internal scattering in CHA and CMA thus providing the electron multiplying effect. Multipliers are
electron spectrometers has been reported in the literature
available in various shapes for both analog and pulse counting
(22-24). amplification modes of operation (31
...
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