ASTM E1078-14(2020)
(Guide)Standard Guide for Specimen Preparation and Mounting in Surface Analysis
Standard Guide for Specimen Preparation and Mounting in Surface Analysis
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.
4.2 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)4 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 any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.
4.4 Guide E1829 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1078 − 14 (Reapproved 2020)
Standard Guide for
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 E1127 Guide for Depth Profiling in Auger Electron Spec-
troscopy
1.1 This guide covers specimen preparation and mounting
E1523 Guide to Charge Control and Charge Referencing
prior to, during, and following surface analysis and applies to
Techniques in X-Ray Photoelectron Spectroscopy
the following surface analysis disciplines:
E1829 Guide for Handling Specimens Prior to Surface
1.1.1 Auger electron spectroscopy (AES),
Analysis
1.1.2 X-ray photoelectron spectroscopy (XPS and ESCA),
2.2 ISO Standards:
and
ISO 18115–1 Surface chemical analysis—Vocabulary—Part
1.1.3 Secondary ion mass spectrometry (SIMS).
1: General terms and terms used in spectroscopy
1.1.4 Although primarily written forAES, XPS, and SIMS,
ISO 18115–2 Surface chemical analysis—Vocabulary—Part
these methods will also apply to many surface sensitive
2: Terms used in scanning-probe microscopy
analysis methods, such as ion scattering spectrometry, low
energy electron diffraction, and electron energy loss
3. Terminology
spectroscopy, where specimen handling can influence surface
sensitive measurements.
3.1 Definitions—For definitions of surface analysis terms
used in this guide, see ISO 18115-1 and ISO 18115-2.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 Proper preparation and mounting of specimens is par-
1.3 This standard does not purport to address all of the
ticularly critical for surface analysis. Improper preparation of
safety concerns, if any, associated with its use. It is the
specimens can result in alteration of the surface composition
responsibility of the user of this standard to establish appro-
and unreliable data. Specimens should be handled carefully so
priate safety, health, and environmental practices and deter-
as to avoid the introduction of spurious contaminants in the
mine the applicability of regulatory limitations prior to use.
preparation and mounting process. The goal must be to
1.4 This international standard was developed in accor-
preserve the state of the surface so that the analysis remains
dance with internationally recognized principles on standard-
representative of the original.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4.2 AES, XPS or ESCA, and SIMS are sensitive to surface
mendations issued by the World Trade Organization Technical layers that are typically a few nanometres thick. Such thin
Barriers to Trade (TBT) Committee. layers can be subject to severe perturbations caused by
specimen handling (1) or surface treatments that may be
2. Referenced Documents
necessary prior to introduction into the analytical chamber. In
addition, specimen mounting techniques have the potential to
2.1 ASTM Standards:
affect the intended analysis.
E983 Guide for Minimizing Unwanted Electron Beam Ef-
fects in Auger Electron Spectroscopy
4.3 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
This guide is under the jurisdiction of ASTM Committee E42 on Surface
described are methods to mount specimens so as to ensure that
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
the desired information is not compromised.
Spectroscopy and X-Ray Photoelectron Spectroscopy.
Current edition approved Dec. 1, 2020. Published December 2020. Originally
approved in 1990. Last previous edition approved in 2014 as E1078 – 14. DOI:
10.1520/E1078-14R20. Available from International Organization for Standardization (ISO), ISO
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Geneva, Switzerland, http://www.iso.org.
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1078 − 14 (2020)
4.4 Guide E1829 describes the handling of surface sensitive 6.1.2 Special caution must be taken with specimens con-
specimens and, as such, complements this guide. taining potential toxins.
6.2 Information Sought—The information sought can influ-
5. General Requirements
ence the preparation of a specimen. If the information sought
5.1 Although the handling techniques for AES, XPS, and comesfromtheexteriorsurfaceofaspecimen,greatercareand
SIMS are basically similar, there are some differences. In precautions in specimen preparation must be taken than if the
general, preparation of specimens for AES and SIMS requires information sought lies beneath an overlayer that must be
more attention because of potential problems with electron or sputtered away in the analytical chamber. Furthermore, it may
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 degree of cleanliness required by surface sensitive
Techniques—It is best if surface analysis measurements are
analyticaltechniquesisoftenmuchgreaterthanforotherforms
made before the specimen is analyzed by other analytical
of analysis.
techniques because such specimens may become damaged or
may be exposed to surface contamination. For example,
5.3 Specimensandmountsmustneverbeincontactwiththe
insulating specimens analyzed by electron microscopy may
bare hand. Handling of the surface to be analyzed should be
have been coated to reduce charging. This coating will render
eliminated or minimized whenever possible. Fingerprints con-
the specimen unsuitable for subsequent surface analysis.
tain mobile species that may contaminate the surface of
Furthermore, exposure to an electron beam (for example, in a
interest. Hand creams, skin oils, and other skin materials are
SEM) can induce damage or cause the adsorption and deposi-
not suitable for high vacuum.
tion of species from the residual vacuum. If it is not possible to
5.4 Visual Inspection:
perform surface analysis first, then the analysis should be done
5.4.1 Avisual inspection should be made, possibly using an
on a different, but nominally identical, specimen or area of the
optical microscope, prior to analysis. At a minimum, a check
specimen.
should be made for residues, particles, fingerprints, adhesives,
contaminants, or other foreign matter.
7. Sources of Specimen Contamination
5.4.2 Features that are visually apparent outside the vacuum
7.1 Tools, Gloves, Etc.:
system may not be observable with the system’s usual imaging
7.1.1 Preparation and mounting of specimens should only
method or through available viewports. It may be necessary to
be done with clean tools to ensure that the specimen surface is
physically mark the specimen outside the area to be analyzed
not altered prior to analysis and that the best possible vacuum
(forexample,withscratchesorapermanentinkmarker)sothat
conditionsaremaintainedintheanalyticalchamber.Toolsused
the analysis location can be found once the specimen is inside
to handle specimens should be made of materials that will not
the vacuum system.
transfer to the specimen or introduce spurious contaminants
5.4.3 Changesthatmayoccurduringanalysismayinfluence
(for example, nickel tools contaminate silicon). Tools should
the data interpretation. Following analysis, visual examination
be cleaned in high purity solvents and dried prior to use.
of the specimen is recommended to look for possible effects of
Nonmagnetic tools should be used if the specimen is suscep-
sputtering, electron beam exposure, X-ray exposure, or
tibletomagneticfields.Toolsshouldneverunnecessarilytouch
vacuum.
the specimen surface.
7.1.2 Although gloves and wiping materials are sometimes
6. Specimen Influences
used to prepare specimens, it is likely that their use may result
6.1 History—The history of a specimen may affect the
in some contamination. Care should be taken to avoid con-
handling of the surface before analysis. For example, a
tamination by talc, silicone compounds, and other materials
specimen that has been exposed to a contaminating environ-
that are often found on gloves. “Powder-free” gloves have no
ment may reduce the need for exceptional care if the surface
talc and may be better suited. Unnecessary contact with the
becomes less reactive. Alternatively, the need for care may
glove or other tool shall be avoided.
increase if the surface becomes toxic.
7.1.3 Specimen mounts and other materials used to hold
6.1.1 If a specimen is known to be contaminated, preclean-
specimens should be cleaned regularly whenever there is a
ing may be warranted in order to expose the surface of interest
possibility of cross-contamination of specimens.Avoid the use
and reduce the risk of vacuum system contamination. If
of tapes containing silicones and other mobile species.
precleaning is desired, a suitable grade solvent should be used
that does not affect the specimen material (electronic grade 7.2 Particulate Debris—Blowing one’s breath on the speci-
solvents if appropriate or available are best suited). Note that men is likely to cause contamination. Compressed gases from
even high purity solvents may leave residues on a surface. aerosol cans or from air lines are often used to blow particles
Cleaning may also be accomplished using an appropriately from the surface or to attempt to clean a specimen. They, too,
filtered pressurized gas. In some instances, the contamination must be considered a source of possible contamination. While
itself may be of interest, for example, where a silicone release particles are removed from specimens by these methods,
agent influences adhesion. In these cases, no precleaning caution is advised and the methods should be avoided in
should be attempted. critical cases. In particular, oil is often a contaminant in
E1078 − 14 (2020)
compressed air lines. In-line particle filters can reduce oil and 7.5.4 In SIMS, atoms sputtered onto the secondary ion
particles from these sources. A gas stream can also produce extractionlensorothernearbysurfacescanberesputteredback
static charge in many specimens, and this could result in onto the surface of the specimen.This effect can be reduced by
attraction of more particulate debris. Use of an ionizing nozzle not having the secondary ion extraction lens or other surfaces
on the gas stream may eliminate this problem. close to the specimen. The use of multiple immersion lens
strips or cleaning of the lens can help reduce this effect.
7.3 Vacuum Conditions and Time—Specimens that were in
7.5.5 The order of use of probing beams can be important,
equilibrium with the ambient environment prior to insertion
especially when dealing with organic material or other fragile
into the vacuum chamber may desorb surface species, such as
materials (such as those discussed in Section 12).
water vapor, plasticizers, and other volatile components. This
may cause cross-contamination of adjacent samples and may
8. Specimen Storage and Transfer
increase the chamber pressure. It also may cause changes in
8.1 Storage:
surface chemistry of the specimens of interest.
8.1.1 Time—The longer a specimen is in storage, the more
7.4 Effects of the Incident Flux:
caremustbetakentoensurethatthesurfacetobeanalyzedhas
7.4.1 The incident electron flux in AES, ion flux in SIMS,
notbeencontaminated.Evenincleanlaboratoryenvironments,
and, to a lesser extent, the photon flux in XPS, may induce
surfaces can quickly become contaminated to the depth ana-
changes in the specimen being analyzed (2), for example by
lyzed byAES, XPS, SIMS, and other surface sensitive analyti-
causing enhanced reactions between the surface of a specimen
cal techniques.
and the residual gases in the analytical chamber. The incident
8.1.2 Containers:
flux also may locally heat or degrade the specimen, or both,
8.1.2.1 Containers suitable for storage should not transfer
resulting in a change of surface chemistry or a possible rise in
contaminants to the specimen by means of particles, liquids,
chamber pressure and in contamination of the analytical
gases, or surface diffusion. Keep in mind unsuitable containers
chamber. These effects are discussed in Guide E983.
may contain volatile species, such as plasticizers, that may be
7.4.2 Residual gases or the incident beam may alter the
emitted, contaminating the surface. Preferably, the surface to
surface. One can test for undesirable effects by monitoring
be analyzed should not contact the container or any other
signalsfromthespecimenasafunctionoftime,forexampleby
object. Glass jars with an inside diameter slightly larger than
setting up the system for a sputter depth profile and then not
the width of a specimen can hold a specimen without contact
turning on the ion gun. If changes with time are observed, then
withthesurface.Whencontactwiththesurfaceisunavoidable,
the interpretation of the results must account for the observa-
wrapping in clean, pre-analyzed aluminum foil may be satis-
tion of an altered surface. This method may also detect
factory. Containers with a beveled bottom may also be appro-
desorption of surface species. Care should be taken to account
priateforstoringflatspecimens(facedowntowardthebevelso
for the possible effects of incident beam fluctuation.
that only the edges of the sample touch the container).
7.4.3 The incident ion beams used during SIMS, AES, and
8.1.2.2 Containers such as glove boxes, vacuum chambers,
XPS depth profiles not only erode the surface of interest but
and desiccators may be excellent choices for storage of
can also affect surfaces nearby. This can be caused by poor
specimens. A vacuum desiccator may be preferable to
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.