ASTM E1078-02

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.
Auger 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 (1)3 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 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: 09-Aug-2002
• 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

Relations

• Replaces: ASTM E1078-97 - Standard Guide for Procedures for Specimen Preparation and Mounting in Surface Analysis
• Effective Date: 10-Aug-2002
• Replaced By: ASTM E1078-09 - Standard Guide for Specimen Preparation and Mounting in Surface Analysis
• Effective Date: 01-May-2009
• Referred By: ASTM E2735-14(2020) - Standard Guide for Selection of Calibrations Needed for X-ray Photoelectron Spectroscopy (XPS) Experiments
• Effective Date: 10-Aug-2002
• Referred By: ASTM E1829-14(2020) - Standard Guide for Handling Specimens Prior to Surface Analysis
• Effective Date: 10-Aug-2002
• Referred By: ASTM F2150-19 - Standard Guide for Characterization and Testing of Biomaterial Scaffolds Used in Regenerative Medicine and Tissue-Engineered Medical Products
• Effective Date: 10-Aug-2002
• Referred By: ASTM F2847-17 - Standard Practice for Reporting and Assessment of Residues on Single-Use Implants and Single-Use Sterile Instruments
• Effective Date: 10-Aug-2002
• Referred By: ASTM E1127-08(2015) - Standard Guide for Depth Profiling in Auger Electron Spectroscopy
• Effective Date: 10-Aug-2002
• Referred By: ASTM E1523-15 - Standard Guide to Charge Control and Charge Referencing Techniques in X-Ray Photoelectron Spectroscopy
• Effective Date: 10-Aug-2002
• Referred By: ASTM E2108-16 - Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer
• Effective Date: 10-Aug-2002
• Referred By: ASTM E996-19 - Standard Practice for Reporting Data in Auger Electron Spectroscopy and X-ray Photoelectron Spectroscopy
• Effective Date: 10-Aug-2002

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
Designation:E1078–02
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope specimens can result in alteration of the surface composition
and unreliable data. Specimens should be handled carefully so
1.1 This guide covers specimen preparation and mounting
as to avoid the introduction of spurious contaminants in the
prior to, during, and following surface analysis and applies to
preparation and mounting process. The goal must be to
the following surface analysis disciplines:
preserve the state of the surface so that the analysis remains
1.1.1 Auger electron spectroscopy (AES),
representative of the original.
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA),
4.2 Auger electron spectroscopy (AES), X-ray photoelec-
and
tron spectroscopy (XPS or ESCA), and secondary ion mass
1.1.3 Secondary ion mass spectrometry, (SIMS).
spectrometry (SIMS) are sensitive to surface layers that are
1.1.4 Although primarily written forAES, XPS, and SIMS,
typically a few nanometers (nm) thick. Such thin layers can be
these methods will also apply to many surface sensitive
subject to severe perturbations caused by specimen handling
analysis methods, such as ion scattering spectrometry, low
3
(1) or surface treatments that may be necessary prior to
energy electron diffraction, and electron energy loss spectros-
introduction into the analytical chamber. In addition, specimen
copy, where specimen handling can influence surface sensitive
mounting techniques have the potential to affect the intended
measurements.
analysis.
1.2 This standard does not purport to address all of the
4.3 This guide describes methods that the surface analyst
safety concerns, if any, associated with its use. It is the
may need to minimize the effects of specimen preparation
responsibility of the user of this standard to establish appro-
when using any surface-sensitive analytical technique. Also
priate safety and health practices and determine the applica-
described are methods to mount specimens so as to ensure that
bility of regulatory limitations prior to use.
the desired information is not compromised.
2. Referenced Documents
4.4 Guide E 1829 describes the handling of surface sensi-
tive specimens and, as such, complements this guide.
2.1 ASTM Standards:
2
E 673 Terminology Relating to Surface Analysis
5. General Requirements
E 983 Guide for Minimizing Unwanted Electron Beam
2
5.1 Although the handling techniques for AES, XPS, and
Effects in Auger Electron Spectroscopy
SIMS are basically similar, there are some differences. In
E 1127 Guide for Depth Profiling in Auger Electron Spec-
2
general, preparation of specimens for AES and SIMS requires
troscopy
more attention because of potential problems with electron or
E 1829 Guide for Handling Specimens Prior to Surface
2
ion beam damage or charging, or both. This guide will note
Analysis
when specimen preparation is significantly different among the
3. Terminology
three techniques.
5.2 The degree of cleanliness required by surface sensitive
3.1 Definitions—For definitions of surface analysis terms
analyticaltechniquesisoftenmuchgreaterthanforotherforms
used in this guide, see Terminology E 673.
of analysis.
4. Significance and Use
5.3 Specimensandmountsmustneverbeincontactwiththe
bare hand. Handling of the surface to be analyzed should be
4.1 Proper preparation and mounting of specimens is par-
eliminated or minimized whenever possible. Fingerprints con-
ticularly critical for surface analysis. Improper preparation of
tain mobile species that may contaminate the surface of
interest.Handcreams,skinoilsandotherskinmaterialsarenot
1
This guide is under the jurisdiction of ASTM Committee E42 on Surface
suitable for high vacuum.
Analysis and is the direct responsibility of Subcommittee E42.03 onAuger Electron
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved August 10, 2002. Published August 2003. Originally
3
approved in 1990. Last previous edition approved in 1997 as E 1078 – 97. The boldface numbers in parentheses refer to the list of references at the end of
2
Annual Book of ASTM Standards, Vol 03.06. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E1078–02
5.4 Visual Inspection: 7. Sources of Specimen Contamination
5.4.1 Avisual inspection should be made, possibly using an
7.1 Tools, Gloves, Etc.:
opti
...