Nanotechnologies - Structural characterization of graphene - Part 1: Graphene from powders and dispersions (ISO/TS 21356-1:2021)

This document specifies the sequence of methods for characterizing the structural properties of graphene, bilayer graphene and graphene nanoplatelets from powders and liquid dispersions using a range of measurement techniques typically after the isolation of individual flakes on a substrate. The properties covered are the number of layers/thickness, the lateral flake size, the level of disorder, layer alignment and the specific surface area. Suggested measurement protocols, sample preparation routines and data analysis for the characterization of graphene from powders and dispersions are given.

Nanotechnologien - Strukturelle Charakterisierung von Graphen - Teil 1: Graphen aus Pulvern und Dispersionen (ISO/TS 21356-1:2021)

Dieses Dokument legt die Abfolge von Verfahren zur Charakterisierung der strukturellen Eigenschaften von Graphen, Zweischicht-Graphen und Graphen-Nanotäfelchen aus Pulvern und flüssigen Dispersionen mittels einer Reihe von Messverfahren, üblicherweise nach der Isolierung einzelner Flocken auf einem Substrat, fest. Zu den erfassten Eigenschaften gehören die Anzahl an Schichten/Dicke, die laterale Flockengröße, der Grad der Unordnung, die Schichtenanordnung und die spezifische Oberfläche. Es werden Vorschläge für Messprotokolle, Probenaufbereitungsabläufe und die Datenanalyse für die Charakterisierung von Graphen aus Pulvern und Dispersionen dargelegt.

Nanotechnologies - Caractérisation structurelle du graphène - Partie 1: Graphène issu de poudres et de dispersions (ISO/TS 21356-1:2021)

Le présent document spécifie la séquence des méthodes qui permettent de caractériser les propriétés structurelles du graphène, du graphène bicouche et des nanoplaquettes de graphène issus de poudres et de dispersions liquides, en utilisant un éventail de techniques de mesure, typiquement après l’isolation de flocons individuels sur un substrat. Les propriétés couvertes sont le nombre de couches/l’épaisseur, la taille latérale du flocon, le niveau de désordre, l’alignement des couches et la surface spécifique. Le présent document suggère également des protocoles de mesure, des modes opératoires pour la préparation des échantillons et des analyses de données pour la caractérisation du graphène issu de poudres et de dispersions.

Nanotehnologije - Strukturne značilnosti grafena - 1. del: Grafen iz prahu in disperzije (ISO/TS 21356-1:2021)

Ta dokument določa zaporedje metod za karakterizacijo strukturnih lastnosti grafena, dvoslojnega grafena ter grafenskih nanoploščic iz prahu in tekoče disperzije z uporabo različnih merilnih tehnik, običajno po izolaciji posameznih kosmov na podlagi. Zajete lastnosti so število slojev/debelina, velikost lateralnih kosmov, stopnja motnje, poravnava slojev in določena površina. Podani so predlogi za protokole merjenja, postopki priprave vzorcev in analizo podatkov za karakterizacijo grafena iz prahu in disperzije.

General Information

Status
Published
Publication Date
22-Mar-2022
Technical Committee
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
23-Mar-2022
Due Date
28-May-2023
Completion Date
23-Mar-2022

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SLOVENSKI STANDARD
01-maj-2022
Nanotehnologije - Strukturne značilnosti grafena - 1. del: Grafen iz prahu in
disperzije (ISO/TS 21356-1:2021)
Nanotechnologies - Structural characterization of graphene - Part 1: Graphene from
powders and dispersions (ISO/TS 21356-1:2021)
Nanotechnologien - Strukturelle Charakterisierung von Graphen - Teil 1: Graphen aus
Pulvern und Dispersionen (ISO/TS 21356-1:2021)
Nanotechnologies - Caractérisation structurelle du graphène - Partie 1: Graphène issu
de poudres et de dispersions (ISO/TS 21356-1:2021)
Ta slovenski standard je istoveten z: CEN ISO/TS 21356-1:2022
ICS:
07.120 Nanotehnologije Nanotechnologies
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN ISO/TS 21356-1
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
March 2022
TECHNISCHE SPEZIFIKATION
ICS 07.120
English Version
Nanotechnologies - Structural characterization of
graphene - Part 1: Graphene from powders and
dispersions (ISO/TS 21356-1:2021)
Nanotechnologies - Caractérisation structurelle du Nanotechnologien - Strukturelle Charakterisierung von
graphène - Partie 1: Graphène issu de poudres et de Graphen - Teil 1: Graphen aus Pulvern und
dispersions (ISO/TS 21356-1:2021) Dispersionen (ISO/TS 21356-1:2021)
This Technical Specification (CEN/TS) was approved by CEN on 13 March 2022 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN ISO/TS 21356-1:2022 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
The text of ISO/TS 21356-1:2021 has been prepared by Technical Committee ISO/TC 229
"Nanotechnologies” of the International Organization for Standardization (ISO) and has been taken over
as CEN ISO/TS 21356-1:2022 by Technical Committee CEN/TC 352 “Nanotechnologies” the secretariat
of which is held by AFNOR.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO/TS 21356-1:2021 has been approved by CEN as CEN ISO/TS 21356-1:2022 without any
modification.
TECHNICAL ISO/TS
SPECIFICATION 21356-1
First edition
2021-03
Nanotechnologies — Structural
characterization of graphene —
Part 1:
Graphene from powders and
dispersions
Nanotechnologies — Caractérisation structurelle du graphène —
Partie 1: Graphène issu de poudres et de dispersions
Reference number
ISO/TS 21356-1:2021(E)
©
ISO 2021
ISO/TS 21356-1:2021(E)
© ISO 2021
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved

ISO/TS 21356-1:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 3
5 Sequence of measurement methods . 3
6 Rapid test for graphitic material using Raman spectroscopy . 5
7 Preparing a liquid dispersion . 7
7.1 General . 7
7.2 Preparing a dispersion of the correct concentration . 7
7.2.1 Powder samples . 7
7.2.2 Samples already in a dispersion . 8
8 Determination of methods . 8
9 Structural characterization using optical microscopy, SEM, AFM and Raman spectroscopy 8
10 Structural characterization using TEM . 9
11 Surface area determination using the BET method .10
12 Graphene lateral size and number fraction calculation .10
Annex A (informative) Rapid test for graphitic material using Raman spectroscopy .11
Annex B (informative) Structural characterization protocol using SEM, AFM and Raman
spectroscopy .14
Annex C (informative) Structural characterization using TEM .29
Annex D (informative) Lateral size and number fraction calculation .36
Annex E (informative) Brunauer–Emmett–Teller method .43
Annex F (informative) Additional sample preparation protocols — Silicon dioxide on
silicon wafer preparation and cleaning .47
Bibliography .48
ISO/TS 21356-1:2021(E)
Foreword
ISO (the International Organization for Standardization) and IEC (the International Electrotechnical
Commission) form the specialized system for worldwide standardization. National bodies that
are members of ISO or IEC participate in the development of International Standards through
technical committees established by the respective organization to deal with particular fields of
technical activity. ISO and IEC technical committees collaborate in fields of mutual interest. Other
international organizations, governmental and non-governmental, in liaison with ISO and IEC, also
take part in the work.
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 document 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 or www .iec .ch/ members
_experts/ refdocs).
Attention is drawn to the possibility that some of the elements of this document may be the subject
of patent rights. ISO and IEC 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) or the IEC
list of patent declarations received (see patents.iec.ch).
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. In the IEC, see www .iec .ch/ understanding -standards.
This document was prepared jointly by Technical Committee ISO/TC 229, Nanotechnologies, and
Technical Committee IEC/TC 113, Nanotechnology for electrotechnical products and systems.
A list of all parts in the ISO/IEC 21356 series can be found on the ISO and IEC websites.
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 and www .iec .ch/ national
-committees.
iv © ISO 2021 – All rights reserved

ISO/TS 21356-1:2021(E)
Introduction
Due to the many superlative properties of graphene and related 2D materials, there are many
application areas where these nanomaterials could be disruptive, areas such as flexible electronics,
nanocomposites, sensing, filtration membranes and energy storage.
There are barriers to commercialisation that are impeding the progress of products containing
graphene, which need to be overcome. One of these crucial barriers is answering the question “What
is my material?”. End-users of the raw materials containing graphene should be able to rely on the
advertised properties of the commercial graphene on the global market, instilling trust and allowing
worldwide trade. Reliable and repeatable measurement protocols are required to address this challenge.
This document provides a set of flow-charts for analysts to follow in order to determine the structural
properties of graphene from powders and liquid dispersions (suspensions). Initially, a quick check
should be undertaken to determine if graphene and/or graphitic material is present. If it is, then further
detailed analysis is required to determine if the sampl
...

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