ASTM E1078-09
(Guide)Standard Guide for Specimen Preparation and Mounting in Surface Analysis
Standard Guide for Specimen Preparation and Mounting in Surface Analysis
SIGNIFICANCE AND USE
Proper preparation and mounting of specimens is particularly critical for surface analysis. Improper preparation of specimens can result in alteration of the surface composition and unreliable data. Specimens should be handled carefully so as to avoid the introduction of spurious contaminants in the preparation and mounting process. The goal must be to preserve the state of the surface so that the analysis remains representative of the original.
AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1) or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.
This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.
Guide E 1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
SCOPE
1.1 This guide covers specimen preparation and mounting prior to, during, and following surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA), and
1.1.3 Secondary ion mass spectrometry, (SIMS).
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will also apply to many surface sensitive analysis methods, such as ion scattering spectrometry, low energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface sensitive measurements.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
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Designation: E1078 − 09
StandardGuide for
1
Specimen Preparation and Mounting in Surface Analysis
This standard is issued under the fixed designation E1078; 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 E1523 Guide to Charge Control and Charge Referencing
Techniques in X-Ray Photoelectron Spectroscopy
1.1 This guide covers specimen preparation and mounting
E1829 Guide for Handling Specimens Prior to Surface
prior to, during, and following surface analysis and applies to
Analysis
the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
3. Terminology
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA),
and 3.1 Definitions—For definitions of surface analysis terms
1.1.3 Secondary ion mass spectrometry (SIMS).
used in this guide, see Terminology E673.
1.1.4 Although primarily written forAES, XPS, and SIMS,
these methods will also apply to many surface sensitive
4. Significance and Use
analysis methods, such as ion scattering spectrometry, low
4.1 Proper preparation and mounting of specimens is par-
energy electron diffraction, and electron energy loss
ticularly critical for surface analysis. Improper preparation of
spectroscopy, where specimen handling can influence surface
specimens can result in alteration of the surface composition
sensitive measurements.
and unreliable data. Specimens should be handled carefully so
1.2 The values stated in SI units are to be regarded as as to avoid the introduction of spurious contaminants in the
standard. No other units of measurement are included in this
preparation and mounting process. The goal must be to
standard. preserve the state of the surface so that the analysis remains
representative of the original.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.2 AES, XPS or ESCA, and SIMS are sensitive to surface
responsibility of the user of this standard to establish appro-
layers that are typically a few nanometres thick. Such thin
priate safety and health practices and determine the applica-
layers can be subject to severe perturbations caused by
4
bility of regulatory limitations prior to use.
specimen handling (1) or surface treatments that may be
necessary prior to introduction into the analytical chamber. In
2. Referenced Documents
addition, specimen mounting techniques have the potential to
2
affect the intended analysis.
2.1 ASTM Standards:
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
4.3 This guide describes methods that the surface analyst
3
2012)
may need to minimize the effects of specimen preparation
E983 Guide for Minimizing Unwanted Electron Beam Ef-
when using any surface-sensitive analytical technique. Also
fects in Auger Electron Spectroscopy
described are methods to mount specimens so as to ensure that
E1127 Guide for Depth Profiling in Auger Electron Spec-
the desired information is not compromised.
troscopy
4.4 Guide E1829 describes the handling of surface sensitive
specimens and, as such, complements this guide.
1
This guide is under the jurisdiction of ASTM Committee E42 on Surface
5. General Requirements
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
5.1 Although the handling techniques for AES, XPS, and
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved May 1, 2009. Published May 2009. Originally
SIMS are basically similar, there are some differences. In
approved in 1990. Last previous edition approved in 2002 as E1078 – 02. DOI:
general, preparation of specimens for AES and SIMS requires
10.1520/E1078-09.
2 more attention because of potential problems with electron or
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.
3 4
The last approved version of this historical standard is referenced on The boldface numbers in parentheses refer to a list of references at the end of
www.astm.org. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E1078 − 09
ion beam damage or charging, or both. This guide will note also be possible to expose the layer of interest by in-situ
when specimen preparation is significantly different among the fracture, cleaving, or other means.
three techniques.
6.3 Specimens Previously Examined by Other Analytical
5.2 The
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E1078–02 Designation:E1078–09
Standard Guide for
1
Specimen Preparation and Mounting in Surface Analysis
This standard is issued under the fixed designation E 1078; 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 This guide covers specimen preparation and mounting prior to, during, and following surface analysis and applies to the
following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA), and
1.1.3 Secondary ion mass spectrometry, (SIMS).
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will also apply to many surface sensitive analysis
methods, such as ion scattering spectrometry, low energy electron diffraction, and electron energy loss spectroscopy, where
specimen handling can influence surface sensitive measurements.
1.2
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E 673 Terminology Relating to Surface Analysis
E 983 Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy
E 1127 Guide for Depth Profiling in Auger Electron Spectroscopy
2
E 1829 Guide for Handling Specimens Prior to Surface Analysis Guide for Handling Specimens Prior to Surface Analysis
E 1523 Guide to Charge Control and Charge Referencing Techniques in X-Ray Photoelectron Spectroscopy
3. Terminology
3.1 Definitions—For definitions of surface analysis terms used in this guide, see Terminology E 673.
4. Significance and Use
4.1 Proper preparation and mounting of specimens is particularly critical for surface analysis. Improper preparation of
specimens can result in alteration of the surface composition and unreliable data. Specimens should be handled carefully so as to
avoid the introduction of spurious contaminants in the preparation and mounting process. The goal must be to preserve the state
of the surface so that the analysis remains representative of the original.
4.2Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS or ESCA), and secondary ion mass
spectrometry (SIMS) are sensitive to surface layers that are typically a few nanometers (nm) thick. Such thin layers can be subject
to severe perturbations caused by specimen handling
4.2 AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers
3
can be subject to severe perturbations caused by specimen handling (1) or surface treatments that may be necessary prior to
introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended
analysis.
4.3 This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using
1
This guide 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 August 10, 2002. Published August 2003. Originally approved in 1990. Last previous edition approved in 1997 as E1078–97.
Current edition approved May 1, 2009. Published May 2009. Originally approved in 1990. Last previous edition approved in 2002 as E 1078 – 02.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book ofASTM Standards
, Vol 03.06.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The boldface numbers in parentheses refer to thea list of references at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E1078–09
any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired
information is not
...
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