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ASTM E1217-05

(Practice)

Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers

Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers

SCOPE
1.1 This practice describes methods for determining the specimen area contributing to the detected signal in Auger electron spectrometers and some types of X-ray photoelectron spectrometers when this area is defined by the electron collection lens and aperture system of the electron energy analyzer. The practice is applicable only to those X-ray photoelectron spectrometers in which the specimen area excited by the incident X-ray beam is larger than the specimen area viewed by the analyzer, in which the photoelectrons travel in a field-free region from the specimen to the analyzer entrance, and in which an auxiliary electron gun can be mounted to produce an electron beam of variable energy on the specimen.
1.2 This practice is recommended as a useful means for determining the specimen area viewed by the analyzer for different conditions of spectrometer operation, for verifying adequate specimen and beam alignment, and for characterizing the imaging properties of the electron energy analyzer.
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

Status
Historical
Publication Date
31-Oct-2005
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
E42 - Surface Analysis
Drafting Committee
E42.03 - Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy
Current Stage
Ref Project

Relations

Replaces
ASTM E1217-00 - Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers
Effective Date
01-Nov-2005
Replaced By
ASTM E1217-11 - Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers
Effective Date
01-Nov-2011
Referred By
ASTM E2735-14(2020) - Standard Guide for Selection of Calibrations Needed for X-ray Photoelectron Spectroscopy (XPS) Experiments
Effective Date
01-Nov-2005
Referred By
ASTM E1016-07(2020) - Standard Guide for Literature Describing Properties of Electrostatic Electron Spectrometers
Effective Date
01-Nov-2005

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ASTM E1217-05 - Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron SpectrometersASTM E1217-05 - Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers
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ASTM E1217-05 - Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers
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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
Designation:E1217–05
Standard Practice for
Determination of the Specimen Area Contributing to the
Detected Signal in Auger Electron Spectrometers and Some
1
X-Ray Photoelectron Spectrometers
This standard is issued under the fixed designation E1217; 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.
3
1. Scope 2.2 ISO Standards:
ISO 18115:2001 Surface Chemical Analysis—Vocabulary
1.1 This practice describes methods for determining the
specimen area contributing to the detected signal in Auger
3. Terminology
electron spectrometers and some types of X-ray photoelectron
3.1 Definitions—See Terminology E673 for terms used in
spectrometers when this area is defined by the electron
AugerelectronspectroscopyandX-rayphotoelectronspectros-
collection lens and aperture system of the electron energy
copy.
analyzer. The practice is applicable only to those X-ray
photoelectron spectrometers in which the specimen area ex-
4. Summary of Practice
cited by the incident X-ray beam is larger than the specimen
4.1 An electron beam with a selected energy is scanned
area viewed by the analyzer, in which the photoelectrons travel
across the surface of a test specimen. The beam may be
in a field-free region from the specimen to the analyzer
scanned once, that is, a line scan, or in a pattern, that is,
entrance, and in which an auxiliary electron gun can be
rastered.As the electron beam is deflected across the specimen
mountedtoproduceanelectronbeamofvariableenergyonthe
surface, measurements are made of the intensities detected by
specimen.
the electron energy analyzer as a function of the beam position
1.2 This practice is recommended as a useful means for
for selected conditions of analyzer operation. The measured
determining the specimen area viewed by the analyzer for
intensities may be due to electrons elastically scattered by the
different conditions of spectrometer operation, for verifying
specimen surface, to electrons inelastically scattered by the
adequate specimen and beam alignment, and for characterizing
specimen, or to Auger electrons emitted by the specimen. The
the imaging properties of the electron energy analyzer.
intensity distributions for a particular detected electron energy
1.3 This standard does not purport to address all of the
can be plotted as a function of beam position in several ways
safety concerns, if any, associated with its use. It is the
and can be utilized to obtain information on the specimen area
responsibility of the user of this standard to establish appro-
contributing to the detected signal and on analyzer perfor-
priate safety and health practices and determine the applica-
mance for the particular conditions of operation. This informa-
bility of regulatory limitations prior to use.
tion can be used to determine the analysis area (see Terminol-
2. Referenced Documents ogy E673 or ISO 18115:2001).
2
2.1 ASTM Standards:
5. Significance and Use
E673 Terminology Relating to Surface Analysis
5.1 Auger electron spectroscopy and X-ray photoelectron
E1016 Guide for Literature Describing Properties of Elec-
spectroscopy are used extensively for the surface analysis of
trostatic Electron Spectrometers
materials. This practice summarizes methods for determining
the specimen area contributing to the detected signal for
instruments in which a focused electron beam can be scanned
1
This practice is under the jurisdiction of ASTM Committee E42 on Surface
over a region with dimensions greater than the dimensions of
Analysis and is the direct responsibility of Subcommittee E42.03 onAuger Electron
the specimen area viewed by the analyzer.
Spectroscopy and X-Ray Photoelectron Spectroscopy.
5.2 This practice is intended as a means for determining the
Current edition approved Nov. 1, 2005. Published December 2005. Originally
approved in 1987. Last previous edition approved in 2000 as E1217 – 00. DOI:
observed specimen area for selected conditions of operation of
10.1520/E1217-05.
the electron energy analyzer. The observed specimen area
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
depends on whether or not the electrons are retarded before
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
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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5.1 Auger electron spectroscopy and X-ray photoelectron spectroscopy are used extensively for the surface analysis of materials. This practice summarizes methods for determining the specimen area contributing to the detected signal (a) for instruments in which a focused electron beam can be scanned over a region with dimensions greater than the dimensions of the specimen area viewed by the analyzer, and (b) by employing a sample with a sharp edge.  
5.2 This practice is intended as a means for determining the observed specimen area for selected conditions of operation of the electron energy analyzer. The observed specimen area depends on whether or not the electrons are retarded before energy analysis, the analyzer pass energy or retarding ratio if the electrons are retarded before energy analysis, the size of selected slits or apertures, and the value of the electron energy to be measured. The observed specimen area depends on these selected conditions of operation and also can depend on the adequacy of alignment of the specimen with respect to the electron energy analyzer.  
5.3 Any changes in the observed specimen area as a function of measurement conditions, for example, electron energy or analyzer pass energy, may need to be known if the specimen materials in regular use have lateral inhomogeneities with dimensions comparable to the dimensions of the specimen area viewed by the analyzer.  
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1.1 This practice describes methods for determining the specimen area contributing to the detected signal in Auger electron spectrometers and some types of X-ray photoelectron spectrometers (spectrometer analysis area) when this area is defined by the electron collection lens and aperture system of the electron energy analyzer. The practice is applicable only to those X-ray photoelectron spectrometers in which the specimen area excited by the incident X-ray beam is larger than the specimen area viewed by the analyzer, in which the photoelectrons travel in a field-free region from the specimen to the analyzer entrance. Some of the methods described here require an auxiliary electron gun mounted to produce an electron beam of variable energy on the specimen (“electron-gun method”). Other experiments require a sample with a sharp edge, such as a wafer covered with a uniform clean layer (for example, gold (Au) or silver (Ag)) and cleaved to obtain a long side (“sharp-edge method”).  
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5.1 Electron multipliers are commonly used in pulse-counting mode to detect ions from magnetic sector mass spectrometers. The electronics used to amplify, detect and count pulses from the electron multipliers always have a characteristic time interval after the detection of a pulse, during which no other pulses can be counted. This characteristic time interval is known as the “dead time.” The dead time has the effect of reducing the measured count rate compared with the “true” count rate.  
5.2 In order to measure count rates accurately over the entire dynamic range of a pulse counting detector, such as an electron multiplier, the dead time of the entire pulse counting system must be well known. Accurate count rate measurement forms the basis of isotopic ratio measurements as well as elemental abundance determinations.  
5.3 The procedure described herein has been successfully used to determine the dead time of counting systems on SIMS instruments.6 The accurate determination of the dead time by this method has been a key component of precision isotopic ratio measurements made by SIMS.
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1.2 This practice is applicable to most types of mass spectrometers that have pulse-counting detectors.  
1.3 This practice does not describe methods for precise or accurate isotopic ratio measurements.  
1.4 This practice does not describe methods for the proper operation of pulse counting systems and detectors for mass spectrometry.  
1.5 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.  
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