ISO/DIS 20579-2

DRAFT INTERNATIONAL STANDARD
ISO/DIS 20579-2
ISO/TC 201/SC 2 Secretariat: ANSI
Voting begins on: Voting terminates on:
2017-08-01 2017-10-23
Surface chemical analysis — Guidelines to sample
handling, preparation and mounting —
Part 2:
Guidelines to preparation and mounting of specimens
prior to analysis
Titre manque —
Partie 2: Titre manque
ICS: 71.040.40
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
This document is circulated as received from the committee secretariat.
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 20579-2:2017(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. ISO 2017
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ISO/DIS 20579-2:2017(E)
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© ISO 2017, Published in Switzerland

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Foreword ..........................................................................................................................................................................................................................................v

Introduction ................................................................................................................................................................................................................................vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Symbols and abbreviated terms ........................................................................................................................................................... 1

5 General requirements ..................................................................................................................................................................................... 1

6 Visual inspection of the specimen ...................................................................................................................................................... 2

7 Specimen considerations ............................................................................................................................................................................. 2

7.1 History ............................................................................................................................................................................................................ 2

7.2 Information sought.............................................................................................................................................................................. 2

7.3 Analysis order with respect to other analytical techniques ............................................................................. 2

8 Sources of specimen contamination ................................................................................................................................................ 3

8.1 Tools, gloves, mounts, and similar materials ................................................................................................................ 3

8.2 Exposure to gases ................................................................................................................................................................................. 3

8.3 Exposure to instrumental vacuum ......................................................................................................................................... 3

8.4 Exposure to electrons, ions, and X-rays ............................................................................................................................. 3

8.5 Contamination of the analytical chamber ........................................................................................................................ 4

9 Specimen storage and transfer .............................................................................................................................................................. 4

9.1 Storage time ............................................................................................................................................................................................... 4

9.2 Storage containers ............................................................................................................................................................................... 4

9.3 Temperature and humidity .......................................................................................................................................................... 4

9.4 Specimen transfer ................................................................................................................................................................................ 5

10 Specimen mounting procedures .......................................................................................................................................................... 5

10.1 General procedures ............................................................................................................................................................................. 5

10.2 Powders and particles ...................................................................................................................................................................... 5

10.3 Wires, fibres, and filaments ......................................................................................................................................................... 6

10.4 Pedestal mounting ............................................................................................................................................................................... 6

10.5 Reduction of thermal damage during analysis ............................................................................................................ 6

11 Methods for reducing specimen charging .................................................................................................................................. 6

11.1 General considerations .................................................................................................................................................................... 6

11.2 Conductive mask, grid, wrap, or coating ........................................................................................................................... 6

11.3 Flood gun ..................................................................................................................................................................................................... 7

11.4 Electron and ion beams ................................................................................................................................................................... 7

11.4.1 Angle of incidence of the primary beam in AES .................................................................................... 7

11.4.2 Energy of the primary beam in AES and SIMS ....................................................................................... 7

11.4.3 Current density of the primary beam in AES and SIMS .................................................................. 7

11.4.4 Combined electron and ion beams in AES ................................................................................................. 7

12 Specimen preparation techniques ..................................................................................................................................................... 7

12.1 General considerations .................................................................................................................................................................... 7

12.2 Mechanical separation...................................................................................................................................................................... 7

12.3 Thinning versus removal ................................................................................................................................................................ 8

12.4 Removal of the substrate ................................................................................................................................................................ 8

12.5 Sectioning techniques ....................................................................................................................................................................... 8

12.5.1 General information ...................................................................................................................................................... 8

12.5.2 Sectioning methods ....................................................................................................................................................... 8

12.5.3 Angle lapping ...................................................................................................................................................................... 8

12.5.4 Ball cratering ....................................................................................................................................................................... 8

12.5.5 Radial sectioning .............................................................................................................................................................. 9

12.5.6 Mechanical polishing ........................................................................................................................................... ......... 9

12.5.7 Chemical and electrochemical polishing ..................................................................................................... 9

12.5.8 Crater edge profiling ..................................................................................................................................................... 9

12.5.9 Focused ion beam sectioning ................................................................................................................................ 9

12.6 Growth of overlayers ......................................................................................................................................................................... 9

12.7 Solvents ......................................................................................................................................................................................................... 9

12.8 Chemical etching ................................................................................................................................................................................10

12.9 Ion sputtering........................................................................................................................................................................................10

12.9.1 General information ...................................................................................................................................................10

12.9.2 Altered layer .....................................................................................................................................................................10

12.9.3 Preferential sputtering ............................................................................................................................................10

12.9.4 Chemical changes .........................................................................................................................................................10

12.9.5 Sputtering with hydrogen .....................................................................................................................................10

12.9.6 Changes of surface and interface topography......................................................................................10

12.9.7 Sputtering and heating ............................................................................................................................................11

12.9.8 Sputter-enhanced diffusion .................................................................................................................................11

12.10 Plasma etching .....................................................................................................................................................................................11

12.11 Heating ........................................................................................................................................................................................................11

12.12 Ultraviolet radiation ........................................................................................................................................................................11

13 Fracturing, cleaving, and scribing ...................................................................................................................................................12

13.1 Fracture ......................................................................................................................................................................................................12

13.1.1 General information ...................................................................................................................................................12

13.1.2 Preparation of specimens .....................................................................................................................................12

13.2 Cleaving ......................................................................................................................................................................................................12

13.3 Scribing .......................................................................................................................................................................................................12

14 Special specimen-handling techniques .....................................................................................................................................13

14.1 Prepumping of gassy specimens ...........................................................................................................................................13

14.2 Viscous liquids ......................................................................................................................................................................................13

14.3 Solute residue .......................................................................................................................................................................................13

Bibliography .............................................................................................................................................................................................................................14

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

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The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

Any trade name used in this document is information given for the convenience of users and does not

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical

Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information

This International Standard is intended to assist analysts and those seeking surface chemical analysis

in the handling, storage, mounting and treatment of specimens. This is a multipart document, with the

first two parts being general requirements for sample handling and storage in ISO 20579-1: Part 1,

and mounting and treatment of samples in ISO 20579-2: Part 2. The ensuing parts combine any new

requirements of sample handling/storage and/or sample mounting/preparation for new materials

classes. Part 3 focuses on biomaterials and Part 4 focuses on reporting needs for nano-objects. Each

part of this international standard can be used independently of the other parts although, the general

procedures described in Parts 1 and 2 are applicable to a wide range of materials and are not reproduced

Although primarily prepared for the surface-analysis techniques of Auger electron spectroscopy (AES),

X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS), the methods

described in this International Standard will also be applicable to many other surface-sensitive

analytical techniques such as ion-scattering spectrometry, scanning probe microscopy, low-energy

electron diffraction and electron energy-loss spectroscopy, where specimen handling can influence

surface-sensitive measurements. AES, XPS and SIMS are sensitive to surface layers that are typically

a few nanometers in thickness. Such thin layers may be subject to severe perturbations caused by

specimen handling or surface treatments that may be necessary prior to introduction into the analytical

chamber. Proper handling and preparation of specimens is particularly critical for dependable analysis.

Improper handling of specimens can result in alteration of the surface composition and unreliable data..

This part of the standard is intended to assist the analyst in understanding the implications of choices

in sample mounting and handling in preparation for analysis. Proper preparation and mounting of

specimens is particularly critical for surface chemical analysis. Improper preparation may result in the

alteration of the surface composition and in unreliable analyses. Specimens shall be handled carefully

so that the introduction of spurious contaminants is avoided or minimized. The goal is to preserve the

state of the surface during preparation and mounting so that the analysis remains representative of

the original specimen. This International Standard describes methods that the surface analyst may

need to use in order to minimize the effects of specimen preparation when using any surface-sensitive

analytical technique. The International Standard also describes methods to mount specimens in order

This International Standard gives guidance on methods of mounting and surface treatment for

a specimen about to undergo surface chemical analysis. It is intended for the analyst as an aid in

understanding the specialized sample-handling conditions required for analyses by techniques such as

Auger electron spectroscopy, secondary-ion mass spectrometry, and X-ray photoelectron spectroscopy.

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

references, the latest edition of the referenced document (including any amendments) applies.

For the purposes of this International Standard, the terms and definitions given in ISO 18115 apply.

General information on sample handling is available in two books. The degree of cleanliness

required by surface-sensitive analytical techniques is much higher than for many other forms of

analysis. Specimens and mounts must never be in contact with the bare hand. Handling of the surface to

be analysed should be eliminated or minimized whenever possible. Fingerprints contain mobile species

that may contaminate the surface of interest. Hand creams, skin oils and other skin materials are not

Although the handling methods for AES, XPS, and SIMS are basically similar, there are some differences.

In general, preparation of specimens for AES and SIMS requires more attention because of potential

problems with electron or ion beam damage or charging, or both. This International Standard will note

A visual inspection of the specimen should be made, possibly using an optical microscope. At a minimum,

a check should be made for residues, particles, fingerprints, adhesives, contaminants or other foreign

Specimen features that are visually apparent when the sample is outside the vacuum system may not be

observable after the sample is placed inside the surface-analysis instrument (for example through use

of any available imaging method or through viewports). It may then be necessary to physically mark

the specimen outside the area to be analysed (e.g. by scribing or by a permanent ink marker) so that the

analysis location can be found once the specimen is inside the vacuum system. Ensure that any method

of marking the sample does not affect the subsequent measurements. Scribing a brittle material may

leave unwanted detritus on the sample that may be deposited in the instrument or that may affect the

analysis. Permanent ink markers may contaminate nearby regions by transport of volatile organics or

Changes that may occur during analysis may influence the data interpretation. Following analysis,

visual examination of the specimen is recommended to look for possible effects of ion-beam sputtering,

electron-beam bombardment, X-ray irradiation, or exposure to the instrumental vacuum.

The history of a specimen may affect the surface before surface analysis. For example, a specimen

that has been exposed to a contaminating environment may become less reactive, and the need for

exceptional care, from an analytical point of view, is then reduced. In such cases, extra care may be

required to meet health and safety requirements. Special caution shall be taken with specimens

If a specimen is known to be contaminated, precleaning may be required to expose the surface of

interest and reduce the risk of vacuum-system contamination. In such cases, the specimen should be

cleaned with a solvent of a suitable grade solvent that is not expected to affect the specimen material.

NOTE Even high-purity solvents can leave residues on a surface. More details on cleaning with solvents are

given in 12.7. In some cases, the contamination may be of interest, e.g. where a silicone-release agent influences

The information sought can influence the preparation of a specimen. If the information sought comes

from the exterior surface of a specimen, greater care and precautions in specimen preparation shall

be taken than if the information sought lies beneath an overlayer that is to be sputtered away in the

analytical chamber. It may also be possible to expose the specimen region of interest by in-situ fracture,

It is preferable for surface chemical analysis measurements to be made before the specimen is

analysed by other techniques because such specimens may become damaged or be exposed to surface

contamination. For example, insulating specimens analysed by electron microscopy may have been

coated to reduce charging. Furthermore, exposure of the specimen to an electron beam (e.g. in a

scanning electron microscope) can induce damage or cause the adsorption of surface species from

the residual vacuum. Such coatings or modifications render the specimen unsuitable for subsequent

surface chemical analysis. If it is not possible to perform the surface chemical analysis first, such an

analysis should be performed on a different, but nominally identical, specimen or area of the specimen.:

Specimens for surface chemical analysis shall be prepared and mounted with clean tools to ensure that

the surface is not altered prior to analysis and that the best possible vacuum conditions are maintained

in the analytical chamber. Tools used to handle specimens should be made of materials that will not

transfer to the specimen (e.g. nickel tools will contaminate silicon). Tools should be cleaned in high-

purity solvents and dried prior to use. Nonmagnetic tools should be used if the specimen is susceptible

to magnetic fields. Tools should not unnecessarily touch the specimen surface to be analysed.

Gloves and wiping materials are sometimes used to handle specimens; it is then likely that their use may

result in some contamination of the specimen surface. Care should be taken to avoid contamination by

talc, silicone compounds, and other materials that are often found on gloves. “Powder-free” gloves have

no talc and may be better suited for use in specimen handling. Unnecessary contact of the specimen

Specimen mounts and other materials used to hold specimens shall be cleaned regularly whenever

there is a possibility of cross-contamination of specimens. The use of tapes containing silicones and

Breathing on the specimen is likely to cause contamination. Compressed gases from aerosol cans or