Nanotechnologies — Clay nanomaterials — Part 2: Specification of characteristics and measurements for clay nanoplates used for gas-barrier film applications

This document specifies characteristics to be measured and measurement methods for clay nanoplate samples in powder and suspension forms used for gas-barrier films. In addition, measurement protocols for the individual characteristics are described. This document does not deal with characteristics of post-manufacturing modification of clay nanoplates. This document does not cover considerations specific to health and safety issues either during manufacturing or use.

Nanotechnologies — Nano argiles — Partie 2: Spécification des caractéristiques et des mesures pour les argiles en nanofeuillets utilisées dans des applications de films barrières aux gaz

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Status
Published
Publication Date
06-May-2021
Current Stage
9093 - International Standard confirmed
Completion Date
08-Oct-2024
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ISO/TS 21236-2:2021 - Nanotechnologies — Clay nanomaterials — Part 2: Specification of characteristics and measurements for clay nanoplates used for gas-barrier film applications Released:5/7/2021
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TECHNICAL ISO/TS
SPECIFICATION 21236-2
First edition
2021-05
Nanotechnologies — Clay
nanomaterials —
Part 2:
Specification of characteristics and
measurements for clay nanoplates
used for gas-barrier film applications
Nanotechnologies — Nano argiles —
Partie 2: Spécification des caractéristiques et des mesures pour
les argiles en nanofeuillets utilisées dans des applications de films
barrières aux gaz
Reference number
©
ISO 2021
© 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

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 2
5 Characteristics and measurement methods . 2
5.1 General . 2
5.2 Mineral composition . 3
5.3 Chemical composition . 3
5.4 Cation exchange capacity . 3
5.5 Particle size . 4
5.6 Loss on ignition . 4
5.7 Methylene blue adsorption capacity . 4
5.8 Aspect ratio . 4
5.9 Film formability. 5
5.10 Viscosity . 5
6 Reporting . 5
Annex A (informative) Measurement protocols . 7
Annex B (informative) Principles of a gas barrier using clay nanoplates .12
Annex C (informative) Value chains of clay nanoplate materials.16
Annex D (informative) Example of reporting sheet .17
Bibliography .18
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 by Technical Committee ISO/TC 229, Nanotechnologies.
A list of all parts in the ISO 21236 series can be found on the ISO website.
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.
iv © ISO 2021 – All rights reserved

Introduction
The barrier property in polymeric materials has become progressively more important in recent years
with the widespread use of plastic films and rigid plastics for food packaging, medical packaging,
electronic devices, construction, agriculture and so on. All polymeric materials have varying degrees
of gas permeability. Therefore, the required level of gas barrier performance varies depending on the
application. Barrier films often consist of multilayers or coated films designed to be impervious to
gas and moisture migration, as single-layer films are in general quite permeable to most gases. Food
packaging films are required to have oxygen gas barrier properties and water vapour barrier properties.
A transparent gas barrier film obtained by applying a silica or alumina vapour deposition method on a
PET or nylon film is generally used for food packaging, pharmaceutical packaging, industrial product
packaging and so on. Recently, a film with a higher level of gas barrier properties has been required for
organic light emitting diode displays. These high gas-barrier properties cannot be achieved by simply
using conventional barrier film for food packaging.
High gas-barrier films are expected to be used in a wide range of fields, such as electronics,
pharmaceutical packaging and hydrogen storage. Various approaches can be taken to improve barrier
properties in plastics packaging. There is a method of adding gas-impermeable nano-objects to plastic
to make nanocomposites. One of the most common types of polymer nanocomposites contains clay
nanoplates. These clay nanomaterials improve barrier properties. Many reports predict the market
expansion of nanocomposite materials.
There are many scientific papers and patents on gas barrier composite material using clay nanoplate.
Gas barrier properties are improved by mixing clay nanoplates into the polymer. The high gas-barrier
phenomenon is described in Nielsen's tortuous model. There are lots of clay products in suspension or
powder forms and the effect of loading is different in each. Different production processes bring various
characteristics to clay-containing materials. Various clay products are available to buy, including
smectite, talc, kaolinite and mica. Some are suitable for gas barrier properties while others are not.
Among them, clay products having a high aspect ratio and high affinity with plastic are preferable.
Users of clay nanoplate products should check the characteristic data described in the catalogue, as
these are important for selecting high-quality clay nanoplates for gas-barrier films.
ISO/TS 21236-1 specifies characteristics of layered clay nanomaterials in powder form, as well as
chemically modified ones, and describes their relevant measurement methods.
This document specifies the characteristics to be measured of clay nanoplate and specifies industrially
available measurement methods used to determine these characteristics. In addition, measurement
protocols are described. It provides a sound basis for the research, development and commercialization
of clay nanoplate materials for the application of barrier films for water vapour and dry gases.
TECHNICAL SPECIFICATION ISO/TS 21236-2:2021(E)
Nanotechnologies — Clay nanomaterials —
Part 2:
Specification of characteristics and measurements for clay
nanoplates used for gas-barrier film applications
1 Scope
This document specifies characteristics to be measured and measurement methods for clay nanoplate
samples in powder and suspension forms used for gas-barrier films. In addition, measurement protocols
for the individual characteristics are described.
This document does not deal with characteristics of post-manufacturing modification of clay
nanoplates. This document does not cover considerations specific to health and safety issues either
during manufacturing or use.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO/TS 80004-6, Nanotechnologies — Vocabulary — Part 6: Nano-object characterization
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO/TS 80004-6 and the following
apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
gas barrier film
film that reduces gas diffusion
3.2
nanoplate
nano-object with one external dimension in the nanoscale and the other two external dimensions
significantly larger
[SOURCE: ISO/TS 80004-2:2015, 4.6, modified]
3.3
clay nanoplate
nanoplate composed of clay
3.4
polymer clay nanocomposite
polymer matrix nanocomposite with a nanostructured clay phase
[SOURCE: ISO/TS 80004-4: 2011, 3.2.1.1]
3.5
film formability
capability of forming a film without additives from a suspension
Note 1 to entry: See Reference [10].
4 Abbreviated terms
AAS atomic absorption spectroscopy
AFM atomic force microscopy
DLS dynamic light scattering
EPMA electron probe micro analysis
ICP inductively coupled plasma spectrometry
SEM-EDX scanning electron microscopy-energy dispersive X-ray spectroscopy
TEM transmission electron microscopy
TGA thermogravimetric analysis
UV-Vis ultraviolet-visible spectrophotometry
XRD X-ray diffraction
XRF X-ray fluorescent analysis
5 Characteristics and measurement methods
5.1 General
The characteristics of clay nanoplate samples to be measured or identified and the applicable
measurement methods are listed in Tables 1 and 2. The characteristics listed in Table 1 shall be
measured by using the listed measurement methods. The characteristics listed in Table 2 should be
measured by using the listed measurement methods. The middle columns in Tables 1 and 2 indicate the
form of test specimen, powder or suspension used for measurements of the individual characteristics.
Test specimens in the specified form are prepared from the suspension or powder sample of clay
nanoplates.
See Annex A for measu
...


TECHNICAL ISO/TS
SPECIFICATION 21236-2
First edition
2021-05
Nanotechnologies — Clay
nanomaterials —
Part 2:
Specification of characteristics and
measurements for clay nanoplates
used for gas-barrier film applications
Nanotechnologies — Nano argiles —
Partie 2: Spécification des caractéristiques et des mesures pour
les argiles en nanofeuillets utilisées dans des applications de films
barrières aux gaz
Reference number
©
ISO 2021
© 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

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 2
5 Characteristics and measurement methods . 2
5.1 General . 2
5.2 Mineral composition . 3
5.3 Chemical composition . 3
5.4 Cation exchange capacity . 3
5.5 Particle size . 4
5.6 Loss on ignition . 4
5.7 Methylene blue adsorption capacity . 4
5.8 Aspect ratio . 4
5.9 Film formability. 5
5.10 Viscosity . 5
6 Reporting . 5
Annex A (informative) Measurement protocols . 7
Annex B (informative) Principles of a gas barrier using clay nanoplates .12
Annex C (informative) Value chains of clay nanoplate materials.16
Annex D (informative) Example of reporting sheet .17
Bibliography .18
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 by Technical Committee ISO/TC 229, Nanotechnologies.
A list of all parts in the ISO 21236 series can be found on the ISO website.
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.
iv © ISO 2021 – All rights reserved

Introduction
The barrier property in polymeric materials has become progressively more important in recent years
with the widespread use of plastic films and rigid plastics for food packaging, medical packaging,
electronic devices, construction, agriculture and so on. All polymeric materials have varying degrees
of gas permeability. Therefore, the required level of gas barrier performance varies depending on the
application. Barrier films often consist of multilayers or coated films designed to be impervious to
gas and moisture migration, as single-layer films are in general quite permeable to most gases. Food
packaging films are required to have oxygen gas barrier properties and water vapour barrier properties.
A transparent gas barrier film obtained by applying a silica or alumina vapour deposition method on a
PET or nylon film is generally used for food packaging, pharmaceutical packaging, industrial product
packaging and so on. Recently, a film with a higher level of gas barrier properties has been required for
organic light emitting diode displays. These high gas-barrier properties cannot be achieved by simply
using conventional barrier film for food packaging.
High gas-barrier films are expected to be used in a wide range of fields, such as electronics,
pharmaceutical packaging and hydrogen storage. Various approaches can be taken to improve barrier
properties in plastics packaging. There is a method of adding gas-impermeable nano-objects to plastic
to make nanocomposites. One of the most common types of polymer nanocomposites contains clay
nanoplates. These clay nanomaterials improve barrier properties. Many reports predict the market
expansion of nanocomposite materials.
There are many scientific papers and patents on gas barrier composite material using clay nanoplate.
Gas barrier properties are improved by mixing clay nanoplates into the polymer. The high gas-barrier
phenomenon is described in Nielsen's tortuous model. There are lots of clay products in suspension or
powder forms and the effect of loading is different in each. Different production processes bring various
characteristics to clay-containing materials. Various clay products are available to buy, including
smectite, talc, kaolinite and mica. Some are suitable for gas barrier properties while others are not.
Among them, clay products having a high aspect ratio and high affinity with plastic are preferable.
Users of clay nanoplate products should check the characteristic data described in the catalogue, as
these are important for selecting high-quality clay nanoplates for gas-barrier films.
ISO/TS 21236-1 specifies characteristics of layered clay nanomaterials in powder form, as well as
chemically modified ones, and describes their relevant measurement methods.
This document specifies the characteristics to be measured of clay nanoplate and specifies industrially
available measurement methods used to determine these characteristics. In addition, measurement
protocols are described. It provides a sound basis for the research, development and commercialization
of clay nanoplate materials for the application of barrier films for water vapour and dry gases.
TECHNICAL SPECIFICATION ISO/TS 21236-2:2021(E)
Nanotechnologies — Clay nanomaterials —
Part 2:
Specification of characteristics and measurements for clay
nanoplates used for gas-barrier film applications
1 Scope
This document specifies characteristics to be measured and measurement methods for clay nanoplate
samples in powder and suspension forms used for gas-barrier films. In addition, measurement protocols
for the individual characteristics are described.
This document does not deal with characteristics of post-manufacturing modification of clay
nanoplates. This document does not cover considerations specific to health and safety issues either
during manufacturing or use.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO/TS 80004-6, Nanotechnologies — Vocabulary — Part 6: Nano-object characterization
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO/TS 80004-6 and the following
apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
gas barrier film
film that reduces gas diffusion
3.2
nanoplate
nano-object with one external dimension in the nanoscale and the other two external dimensions
significantly larger
[SOURCE: ISO/TS 80004-2:2015, 4.6, modified]
3.3
clay nanoplate
nanoplate composed of clay
3.4
polymer clay nanocomposite
polymer matrix nanocomposite with a nanostructured clay phase
[SOURCE: ISO/TS 80004-4: 2011, 3.2.1.1]
3.5
film formability
capability of forming a film without additives from a suspension
Note 1 to entry: See Reference [10].
4 Abbreviated terms
AAS atomic absorption spectroscopy
AFM atomic force microscopy
DLS dynamic light scattering
EPMA electron probe micro analysis
ICP inductively coupled plasma spectrometry
SEM-EDX scanning electron microscopy-energy dispersive X-ray spectroscopy
TEM transmission electron microscopy
TGA thermogravimetric analysis
UV-Vis ultraviolet-visible spectrophotometry
XRD X-ray diffraction
XRF X-ray fluorescent analysis
5 Characteristics and measurement methods
5.1 General
The characteristics of clay nanoplate samples to be measured or identified and the applicable
measurement methods are listed in Tables 1 and 2. The characteristics listed in Table 1 shall be
measured by using the listed measurement methods. The characteristics listed in Table 2 should be
measured by using the listed measurement methods. The middle columns in Tables 1 and 2 indicate the
form of test specimen, powder or suspension used for measurements of the individual characteristics.
Test specimens in the specified form are prepared from the suspension or powder sample of clay
nanoplates.
See Annex A for measu
...

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