ISO TS 22292:2021

Nanotechnologies – 3D image reconstruction of rod-supported nano-objects using transmission electron microscopy

ISO TS 22292:2021 This document provides guidance for sample preparation, data acquisition by transmission electron microscopy, data processing, and three-dimensional image reconstruction to measure size and shape parameters of nano-objects on rod-shaped supports. The method is applicable to samples dispersed on or within an electron-transparent rod-shaped support.

General Information

• Status: Published
• Publication Date: 13-Jun-2021
• ICS: 07.120 - Nanotechnologies
• ICS: 37.020 - Optical equipment
• Technical Committee: TC 113 - Nanotechnology for electrotechnical products and systems
• Drafting Committee: JWG 2 - TC 113/JWG 2
• Current Stage: PPUB - Publication issued
• Start Date: 05-May-2022
• Completion Date: 25-Mar-2022

Standards Content (Sample)

TECHNICAL ISO/TS
SPECIFICATION 22292
First edition
2021-06
Nanotechnologies — 3D image
reconstruction of rod-supported nano-
objects using transmission electron
microscopy
Nanotechnologies — Reconstruction d'images 3D de nano-objets
soutenus par des tiges à l'aide de la microscopie électronique à
transmission
Reference number
ISO/TS 22292:2021(E)
©
ISO 2021
ISO/TS 22292:2021(E)
© ISO 2021
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
ii © ISO 2021 – All rights reserved

ISO/TS 22292:2021(E)
Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
3.1 Nanotechnology-related terms . 2
3.2 Instrument-related terms . 2
3.3 Measurement-related terms. 3
4 Sample considerations . 4
4.1 General . 4
4.2 Choice of sample rod diameter . 4
5 Instrument factors . 4
5.1 Microscope set up . 4
5.1.1 General. 4
5.1.2 Acceleration voltage . . 5
5.1.3 Convergence semi-angle . 5
5.1.4 Collection angle . 5
5.1.5 Microscope magnification . 5
5.1.6 Number of pixels of the detector . 5
5.1.7 Image acquisition time . 6
5.2 Microscope calibration . 6
6 Image capture (data acquisition) . 7
6.1 General . 7
6.2 Procedure . 7
7 Data alignment and volume reconstruction .10
7.1 General .10
7.2 Procedure .10
8 Reconstructed volume evaluation and data analysis .10
8.1 General .10
8.2 Identification of nanoparticles and 3D volume .10
8.3 Thresholding for measurand extraction .11
9 Expression of results .13
9.1 Extracting parameters for each well-separated nano-object.13
9.2 Measurement uncertainty .14
9.3 Sources of errors .14
9.3.1 Error arising from sample that is not representative of the object of interest .14
9.3.2 Acquisition of 2D projected images .14
9.3.3 Instrument calibration . .16
9.3.4 Alignment of the projected images .16
9.3.5 Reconstruction of the 3D volume .16
9.3.6 Discrete representation of the objects (nanoparticles) in 3D .16
9.3.7 Interpretation of the obtained measurands .17
9.3.8 Limited number of observed objects (nanoparticles) .17
10 Test report .19
Annex A (informative) Sample preparation .21
Annex B (informative) STEM set up .28
Annex C (normative) Tomography reconstruction and visualization software packages .30
Annex D (informative) Microscope data collection parameters .32
ISO/TS 22292:2021(E)
Annex E (informative) Case study: Metal nanoparticle, ILC results .33
Annex F (informative) Case study — Organic nanoparticles — Sample preparation and use.38
Annex G (informative) Particle distortions arising from FBP and SIRT reconstruction methods .39
Annex H (informative) Uncertainty budget .41
Bibliography .43
iv © ISO 2021 – All rights reserved

ISO/TS 22292:2021(E)
Foreword
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
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
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
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
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
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/
iso/ foreword .html.
This document was prepared jointly by Technical Committee ISO/TC 229, Nanotechnologies, and
Technical Committee IEC/TC 113, Nanotechnology for electrotechnical products and systems.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
ISO/TS 22292:2021(E)
Introduction
Electron tomography, in transmission electron microscope (TEM), has impact on nanotechnology
and nanomaterial metrology like that of computer tomography in medicine. For example, industries
using nanotechnologies have requirements to verify materials, processes and products. Quantitative
measurement at the nanoscale, including three-dimensional (3D) image reconstruction of nano-objects
using TEM, responds to this need.
TEM, a two-dimensional (2D) imaging instrument, can provide 2D projection images of materials at
the nanoscale, in the length range from below 1 nm to above 100 nm. From multiple 2D TEM images
collected at suitable tilt increments, the 3D shape, size and volume parameters can be determined. This
document describes sample preparation, instrumentation setup, data acquisition and processing for
3D image reconstruction of nano-objects using TEM, from which dimensional parameter values can
be determined and interpreted. Variation in methodology for use with scanning transmission electron
microscopy (STEM) is included in an informative annex.
The method described herein is limited to samples dispersed on or within an electron-transparent
rod-shaped support. This method is particularly useful when the detailed shape of a limited number
of objects, such as nanoparticles, is sought. For example, when 2D measurements yield a non-uniform
distribution of objects, 3D image reconstruction can be used applied to study a small number of the
objects in more detail. A variant of sample preparation is described that allows 3D reconstruction to
be used in conjun
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