ASTM E1829-14(2020)

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: E1829 − 14 (Reapproved 2020)
Standard Guide for
Handling Specimens Prior to Surface Analysis
This standard is issued under the fixed designation E1829; 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 2.2 ISO Standards:
ISO 18115-1 Surface chemical analysis—Vocabulary—Part
1.1 This guide covers specimen handling and preparation
1: General terms and terms used in spectroscopy
prior to surface analysis and applies to the following surface
ISO 18115-2 Surface chemical analysis—Vocabulary—Part
analysis disciplines:
2: Terms used in scanning-probe microscopy
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA),
3. Terminology
and
3.1 Definitions—For definitions of surface analysis terms
1.1.3 Secondary ion mass spectrometry (SIMS).
used in this guide, see ISO 18115-1 and ISO 18115-2.
1.1.4 Although primarily written forAES, XPS, and SIMS,
these methods may also apply to many surface-sensitive
4. Significance and Use
analysis methods, such as ion scattering spectrometry, low-
4.1 Proper handling and preparation of specimens is par-
energy electron diffraction, and electron energy loss
ticularly critical for analysis. Improper handling of specimens
spectroscopy, where specimen handling can influence surface-
can result in alteration of the surface composition and unreli-
sensitive measurements.
abledata.Specimensshouldbehandledcarefullysoastoavoid
1.2 This standard does not purport to address all of the
the introduction of spurious contaminants. The goal must be to
safety concerns, if any, associated with its use. It is the
preserve the state of the surface so that analysis remains
responsibility of the user of this standard to establish appro-
representative of the original subject.
priate safety, health, and environmental practices and deter-
4.2 AES, XPS, and SIMS are sensitive to surface layers that
mine the applicability of regulatory limitations prior to use.
are typically a few nanometres thick. Such thin layers can be
1.3 This international standard was developed in accor-
subject to severe perturbations from improper specimen han-
dance with internationally recognized principles on standard-
dling (1).
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4.3 This guide describes methods to minimize the effects of
mendations issued by the World Trade Organization Technical
specimen handling on the results obtained using surface-
Barriers to Trade (TBT) Committee.
sensitive analytical techniques. It is intended for the specimen
owner or the purchaser of surface analytical services and the
2. Referenced Documents
surface analyst. Because of the wide range of types of
2.1 ASTM Standards:
specimens and desired information, only broad guidelines and
E1078 Guide for Specimen Preparation and Mounting in
general examples are presented here. The optimum handling
Surface Analysis
procedures will be dependent on the particular specimen and
the needed information. It is recommended that the specimen
supplier consult the surface analyst as soon as possible with
This guide is under the jurisdiction of ASTM Committee E42 on Surface
regardtospecimenhistory,thespecificproblemtobesolvedor
Analysis and is the direct responsibility of Subcommittee E42.03 on Auger Electron
Spectroscopy and X-Ray Photoelectron Spectroscopy. information needed, and the particular specimen preparation or
Current edition approved Dec. 1, 2020. Published December 2020. Originally
approved in 1996. Last previous edition approved in 2014 as E1829 – 14. DOI:
10.1520/E1829-14R20. 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
E1829 − 14 (2020)
handling procedures required. The surface analyst also is 6.3 Specimens Previously Examined by Other Analytical
referred to Guide E1078 that discusses additional procedures Techniques—It is best if surface analysis measurements are
for preparing, mounting, and analysis of specimens. made before the specimen is analyzed by other analytical
techniques because such specimens may become damaged or
may be exposed to surface contamination. For example,
5. General Requirements
insulating specimens analyzed by electron microscopy may
5.1 The degree of cleanliness required by surface-sensitive
have been coated to reduce charging. This coating renders the
analyticaltechniquesoftenismuchgreaterthanforotherforms
specimens unsuitable for subsequent surface analysis. Expo-
of analysis.
sure to an electron beam (for example, in a SEM) also can
5.2 Specimens must never be in contact with the bare hand.
induce damage or deposit additional contamination. If it is not
Handling of the surface to be analyzed should be eliminated or
possible to perform the surface analysis work first, then the
minimized whenever possible.
analysis should be done on a different, but nominally identical,
specimen or area of the specimen.
5.3 Specimens should be transported to the analyst in a
container that does not come into direct contact with the
6.4 Information Sought—Surface chemical analysis can be
surface of interest.
performed on a wide range of specimens and can be used to
obtain very different types of information about surfaces or
5.4 In most cases, the analysis will be performed on the “as
interfaces. The degree of care that must to be taken depends
received” specimen. Surface contamination or atmospheric
upon the type of analysis that is required and the nature of the
adsorbates are not usually removed because of the importance
problem. The information being sought usually falls into three
of analyzing an unaltered surface and as these are often the
general categories: (Type A) information on the outermost
regions of interest. Care must then be taken in handling the
surface; (Type B) information as a function of depth (depth
specimen to ensure that no outside agents come in contact with
profile) or at a buried interface; and (Type C) information that
thesurfacetobeinvestigated.Theseagentsinclude:solventsor
will require subsequent specimen preparation by the analyst.
cleaning solutions, gases (including compressed air) or vapors,
6.4.1 TypeAspecimens include those to be investigated for
metals, tissue or other wrapping materials, tape, cloth, tools,
surface contamination, surface stains, and adhesion failures.
packing materials, or the walls of containers. If the specimen
This category requires the most care in preparation and
supplier is uncertain of the requirements for a specific
packaging. Ideally, nothing should be allowed to contact the
specimen, they should consult the analyst.
surface of interest. In practice, it may be necessary to wrap the
5.5 In some cases (for example, for a large specimen), it
samples to avoid damage in transit. (See Appendix X3.)
may be necessary to take a representative sample from the
6.4.2 Type B specimens include those that require the
specimen. Selection of a smaller sample from a larger speci-
investigation of thick and thin films, single layers, multilayers,
men should be done while considering the information being
metal contact layers on semiconductors, coatings, dopant
sought because inhomogeneities are often present. It is recom-
profiles, and the chemical and physical properties at an
mended that this choice be made in consultation with an
interface between two dissimilar materials. For this category,
experienced analyst.
the packaging requirements are not as stringent although care
5.6 Numerousmethodsexistforthemountingofaspecimen
should still be taken to not contaminate the specimen. In this
in preparation for analysis. Refer to Guide E1078.
class, the information sought comes from a layer below the
outermost surface and superficial surface contamination is not
5.7 Hazardous Materials—Special caution shall be exer-
an issue. With semiconductor samples, care should be taken to
cised with specimens containing potential toxins or other
avoid particulate contamination of the surface as this can
hazardous materials. Whenever possible, chemical hazard data
degrade the quality of the depth profiles.
sheets should be supplied with the specimen.
6.4.3 Type C specimens include those that require prepara-
5.8 The severity of the requirement for specimen handling
tion by the analyst and includes specimens for in-situ fracture,
varies dramatically with the condition of the surface and the
metallurgical lapping or polishing, and specimens that are part
location of the information being sought. The list in Appendix
of a larger assembly. Generally, these specimens must be
X1 describes types of specimens by their increasing sensitivity
shaped (for example, for fracture), chemically or mechanically
to handling.
altered (as happens with lapping) or disassembled. Few special
precautions are needed for samples that are to be fractured, or
6. Specimen Influences
undergo further sample preparation by the analyst. For speci-
6.1 The analyst should be advised of the specimen history, men in a larger assembly or subassembly, it may be preferable
special storage or transport requirements, exposure to possible to leave the specimen in place and let the analyst remove it for
contaminants, and the information being sought. analysis. Nonetheless, care should still be taken to not con-
taminate the specimen.
6.2 History—The history of a specimen can influence the
handling of its surface. For example, a specimen that has been 6.5 Clearly identify all specimens with a unique name or
previously exposed to a contaminating environment may identifier.Ifitispossibletopermanentlyattachthisidentifierto
reducetheneedforexceptionalcareifthesurfacebecomesless the specimen (without disturbing the area of interest), do so.
reactive. Alternatively, the need for care may increase if the Clearly indicate the area of analysis by marking up a drawing
surface becomes toxic. oraphotograph.Ifnecessary,ascribeorpermanentinkmarker
E1829 − 14 (2020)
can be used on an area adjacent to the areas of interest. If there surfaces can become contaminated quickly to the depth ana-
isanydoubtastowhichsideofthespecimenistobeanalyzed, lyzed byAES, XPS, SIMS, and other surface sensitive analyti-
clearly mark the back of the specimen. cal techniques.
8.1.2 Containers:
6.6 Precautions—Donottouchthesurfaceofinterest,either
8.1.2.1 Containers suitable for storage should not transfer
by hand or with a tool. Do not “protect” the surface of interest
contaminants to the specimen by means of particles, liquids,
by covering it with tape, contaminated foil or porous wrapping
gases, or surface diffusion. Keep in mind that volatile species
material.Donotuseadiamondscribetomarksemiconductors.
(for example, plasticizers) may be emitted from such
Fragile specimens should not be mounted onto double-sided
containers, further contaminating the surface. Preferably, the
tape.
surface to be analyzed should not contact the container or any
other object. Glass jars with an inside diameter slightly larger
7. Sources of Specimen Contamination
than the width of a specimen can hold a specimen without
7.1 An unprotected hand must never handle specimens,
contact with the surface. When contact with the surface is
even when the skin will not touch the surface of interest.
unavoidable, wrapping in clean, pre-analyzed aluminum foil
Fingerprints and hand creams contain mobile species that may
may be satisfactory. For semiconductor samples, standard
migrate and contaminate the surface of interest.
wafer carriers are generally adequate.
7.2 Handling of specimens only should be done with clean
8.1.2.2 Containers, such as glove boxes, vacuum chambers,
tools to ensure that the specimen surface is not altered prior to
and desiccators may be excellent cho
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