ASTM E1829-97
(Guide)Standard Guide for Handling Specimens Prior to Surface Analysis
Standard Guide for Handling Specimens Prior to Surface Analysis
SCOPE
1.1 This guide covers specimen handling and preparation prior to 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 or ESCA), and
1.1.3 Secondary ion mass spectrometry, SIMS.
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may 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.
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Designation: E 1829 – 97
Standard Guide for
Handling Specimens Prior to Surface Analysis
This standard is issued under the fixed designation E 1829; 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 4.2 Auger electron spectroscopy, X-ray photoelectron spec-
troscopy, and secondary ion mass spectroscopy are sensitive to
1.1 This guide covers specimen handling and preparation
surface layers that are typically a few nanometres in thickness.
prior to surface analysis and applies to the following surface
Such thin layers can be subject to severe perturbations from
analysis disciplines:
improper specimen handling (1).
1.1.1 Auger electron spectroscopy (AES),
4.3 This guide describes methods to minimize the effects of
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA),
specimen handling and preparation on the results obtained
and
using surface-sensitive analytical techniques. It is intended for
1.1.3 Secondary ion mass spectrometry, SIMS.
the specimen owner or the purchaser of surface analytical
1.1.4 Although primarily written for AES, XPS, and SIMS,
services and the surface analyst. Because of the wide range of
methods also will apply to many surface-sensitive analysis
types of specimens and desired information, only broad guide-
methods, such as ion scattering spectrometry, low-energy
lines and specific examples are presented here. The optimum
electron diffraction, and electron energy loss spectroscopy,
handling procedures will be dependent on the particular
where specimen handling can influence surface-sensitive mea-
specimen and the needed information. It is recommended that
surements.
the specimen preparer or owner consult the surface analyst as
1.2 This standard does not purport to address all of the
soon as possible with regard to specimen history, specific
safety concerns, if any, associated with its use. It is the
problem to be solved or information needed, and particular
responsibility of the user of this standard to establish appro-
specimen preparation or handling procedures required. The
priate safety and health practices and determine the applica-
surface analyst also is referred to Guide E 1078 that discusses
bility of regulatory limitations prior to use.
additional procedures for preparing, mounting, and analysis of
2. Referenced Documents
specimens.
2.1 ASTM Standards:
5. General Requirements
E 673 Terminology Relating to Surface Analysis
5.1 The degree of cleanliness required by surface-sensitive
E 1078 Guide for Specimen Preparation and Mounting in
analytical techniques often is much greater than for other forms
Surface Analysis
of analysis. Scientists, engineers, and managers new to AES,
3. Terminology XPS, and SIMS often need to be educated regarding these
more stringent requirements.
3.1 Definitions—For definitions of surface analysis terms
5.2 Contact—Any handling of the surface area to be ana-
used in this guide, see Terminology E 673. Specimens should
lyzed should be eliminated or minimized whenever possible.
be handled carefully so as to avoid the introduction of spurious
5.3 Hazardous Materials—Special caution should be exer-
contaminants. The goal must be to preserve the state of the
cised with specimens containing potential toxins or other
surface so that analysis remains representative of the original
hazardous materials.
subject.
6. Specimen Influences
4. Significance and Use
6.1 History—The history of a specimen can influence the
4.1 Proper handling and preparation of specimens is par-
handling of its surface. For example, if a specimen previously
ticularly critical for analysis. Improper handling of specimens
has been exposed to a contaminating environment, the need for
can result in alteration of the surface composition, which
exceptional care in handling might be less than for a specimen
results in erroneous data.
that came from a very clean environment.
6.2 Information Sought—The information sought can influ-
This guide is under the jurisdiction of ASTM Committee E-42 on Surface ence the handling of a specimen. If the information sought lies
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
Spectroscopy and X-ray Photoelectron Spectroscopy.
Current edition approved Sept. 10, 1997. Published June 1998. Originally
published as E 1829 – 96. Last previous edition E 1829 – 96. The boldface numbers in parentheses refer to the list of references at the end of
Annual Book of ASTM Standards, Vol 03.06. this standard.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1829
beneath an overlayer that must be sputtered away in the 8.1.2.1 Containers suitable for storage should not transfer
analytical chamber, or can be exposed by in situ fracture, contaminants to the specimen by means of particles, liquids,
cleaving, or other means, then more handling may be allowed gases, or surface diffusion. Keep in mind that volatile species
than if the information sought comes from the exterior surface such as plasticizers may be emitted from such containers,
of a specimen. further contaminating the surface. Preferably, the surface to be
6.3 Specimens Previously Examined by Other Analytical analyzed should not contact the container or any other object.
Techniques—Information available from other analytical tech- Glass jars with an inside diameter slightly larger than the width
niques can influence the selection of surface-sensitive measure- of a specimen can hold a specimen without contact with the
ments and handling of a specimen. Specimens that have been surface. When contact with the surface is unavoidable, wrap-
analyzed previously may be contaminated on their surfaces. In ping in clean, preanalyzed aluminum foil may be satisfactory.
particular, specimens examined in an electron microscope For semiconductor samples, standard wafer carriers are gener-
typically have been coated to reduce charging. This thick ally adequate.
coating renders the specimens unsuitable for subsequent sur- 8.1.2.2 Containers, such as glove boxes, vacuum chambers,
face analysis, although surface composition information can be and desiccators may be excellent choices for storage of
obtained by sputtering through the overlayer. The electron specimens. A vacuum desiccator may be preferable to a
beam in an SEM also can induce damage or deposit additional standard unit and should have been maintained free of grease
contamination. In general, it is best to perform surface analysis and mechanical pump oil. Cross contamination
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